Brief introduction of 763111-47-3

The synthetic route of 763111-47-3 has been constantly updated, and we look forward to future research findings.

763111-47-3, 4-(4-Fluoro-3-(piperazine-1-carbonyl)benzyl)phthalazin-1(2H)-one is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A QMA cartridge containing cyclotron -produced [18F] fluoride ion was euted with a solution containing 9 mg Kryptofix [2.2,2] (4,7.13, 16,21,24- hexaoxa- l,10-diaza bicycloi8.8.8]hexacosane), 0.08 m L 0.15 M K2C03 and 1.92 m L MeCN into a 5 m L reaction vial. Water was removed azeotropically at 120 C. 500 mug of ethyl 4-nitrobenzoate dissolved in 100 mu of DMSO was then added to the reaction vial and heated to 150 C for 15 minutes. The reaction via l was then allowed to cool as 50 mu of 1M NaOH was added. The reaction mixture was stirred for 1 min and 50 mu of 1M HCI was added to quench. Then, 2 mg of 4-(4-fiuoro-3-(piperazine-l-carbonyl)benzyi)phthaiazin- l(2H)-one dissolved in 100 mu of DMSO was added , followed by 10 mg of HBT U dissolved in 100 mu of DMSO and 20 mu. of Et3N. The reaction mixture was stirred for 1 minute. 400 mu MeCN followed by 700 mu H20 was then added and the solution was injected onto a C6-Pheny analytical HPLC column and eluted under isocratic conditions (Method B: 30% acetonitrile in water for 35min). Compound C- 2f eluted at (tR = 25.5 min), which was well resolved from the nitro analogue (4-(4-fluoro-3-(4-(4- nitrobenzoyl)piperazine-l-carbonyl)benzyl)phthalazin-l(2H)-one; tR = 30.1 min). For intravenous administration, the product-containing fraction was passed through a CIS light-SepPak cartridge preconditioned with EtOH (10 m L) and water (10 mL). The cartridge was washed with water (3 m L) and C-2f was eluted using EtOH (400 mu). The solution was then diluted with 0.9% saline to 10% EtOH. The radiochemical purity of the final formulation was confirmed using analytical HPLC.

The synthetic route of 763111-47-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; MEMORIAL SLOAN KETTERING CANCER CENTER; REINER, Thomas; LEWIS, Jason S.; WEBER, Wolfgang; RODRIGUEZ, Beatriz Salinas; CARNEY, Brandon; CARLUCCI, Giuseppe; (89 pag.)WO2016/33293; (2016); A1;,
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Some tips on 89898-86-2

89898-86-2 5-Nitrophthalazine 11105874, aphthalazine compound, is more and more widely used in various.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.89898-86-2,5-Nitrophthalazine,as a common compound, the synthetic route is as follows.

To 0.88g (5.0mmol) of 5-nitrophthalazine in 30mL of tetrahydrofuran at 50C was added 4.37g (25.1mmol) of sodium hydrogen sulfite in 15mL of water. The reaction mixture was stirred at 50C for 15min. The organic solution was extracted with ethyl acetate (3¡Á100mL), washed with brine (50mL), and dried over magnesium sulfate. Filtration and removal of the solvent under reduced pressure gave the product as a bright yellow precipitate. The precipitate was recrystallized in a hot methanol solution to afford 0.49g (67%) of 5-aminophthalazine. 1H NMR (400MHz, DMSO-d6) delta: 9.80 (s, 1H), 9.60 (s, 1H), 7.60 (dd, J=4. 6, 7.6Hz, 1H), 7.20 (dd, J=1.9, 4.6Hz, 1H), 7.02 (d, J=7.6Hz, 1H), 6.50 (s, 2H). 13C NMR (100.17MHz, DMSO-d6) delta: 150.1, 146.5, 145.1, 133.2, 126.1, 114.7, 114.1, 112.2.

89898-86-2 5-Nitrophthalazine 11105874, aphthalazine compound, is more and more widely used in various.

Reference£º
Article; Paige, Mikell; Kosturko, George; Bulut, Guellay; Miessau, Matthew; Rahim, Said; Toretsky, Jeffrey A.; Brown, Milton L.; Ueren, Aykut; Bioorganic and Medicinal Chemistry; vol. 22; 1; (2014); p. 478 – 487;,
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Brief introduction of 763111-47-3

The synthetic route of 763111-47-3 has been constantly updated, and we look forward to future research findings.

763111-47-3, 4-(4-Fluoro-3-(piperazine-1-carbonyl)benzyl)phthalazin-1(2H)-one is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

4-(4-Fluoro-3-(piperazin-1-yl-carbonyl)-benzyl)pyridazine-1(2H)one (5) (1.56 g, 4.26 mmol) was added to a 25 ml three-necked flask.And added dichloromethane (6.5 ml), trans-4-dimethylamino crotonic acid (0.78 g, 6.04 mmol),HOBT (0.87 g, 6.44 mmol), EDCI (1.23 g, 6.42 mmol), and then cooled to 0-10 C, then DIPEA (4.42 g, 34.3 mmol) was added dropwise, and the mixture was allowed to warm to room temperature and stirred for 2 h.After TLC showed that the reaction was completed, the reaction mixture was quenched with water (30 mL).The solid crude product was added to the acid water, the impurities were extracted with dichloromethane, the aqueous phase was made alkaline, and the product was extracted with dichloromethane (20 mL¡Á3);The combined organic phases were dried over anhydrous sodium sulfate, filtered and evaporatedThe white solid product was then beaten with n-hexane (5 ml).Filter and dry to give 470 mg of a white solid.The yield was 23%.

The synthetic route of 763111-47-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Shanghai Bobang Pharmaceutical Technology Co., Ltd.; Gao Heyong; Liu Zhende; Zhang Wensheng; (28 pag.)CN108383798; (2018); A;,
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Simple exploration of 76240-49-8

76240-49-8 6-Bromophthalazine-1,4-diol 11379478, aphthalazine compound, is more and more widely used in various.

76240-49-8, 6-Bromophthalazine-1,4-diol is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of 6-bromo-2,3-dihydrophthalazine-1,4-dione (CAS 76240-49-8, 36.0 g, 150 mmol) and Et3N (37.5 g, 375 mmol) in DCM (1.0 L) was added Tf20 (42.3 g, 150 mol) dropwise over 1 h. The mixture was stirred at 0 C for 2 h and then kept at 15 C for 16 h. The mixture was filtered and the filtrate was concentrated. The residue was purified by flash column(petroleum ether: EtOAc from 5:1 to 3:1) to give a mixture of the title compounds (9.0 g, 16% yield) as a white solid.

76240-49-8 6-Bromophthalazine-1,4-diol 11379478, aphthalazine compound, is more and more widely used in various.

Reference£º
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; CUMMING, John G.; LIN, Xianfeng; LIU, Haixia; NAJERA, Isabel; QIU, Zongxing; SANDRIN, Virginie; TANG, Guozhi; WU, Guolong; (204 pag.)WO2018/1948; (2018); A1;,
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New learning discoveries about 1242156-59-7

As the paragraph descriping shows that 1242156-59-7 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1242156-59-7,6-(tert-Butyl)-8-fluorophthalazin-1(2H)-one,as a common compound, the synthetic route is as follows.

Example 102b 2-Bromo-6-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)-4-fluorobenzaldehyde 102b To a solution of 102a (767 mg, 2.72 mmol), 6-tert-butyl-8-fluorophthalazin-1(2H)-one 101h (300 mg, 1.36 mmol) in dioxane (50 mL) was added KOAc (267 mg, 2.72 mmol), CuI (259 mg, 1.36 mmol), and 4,7-dimethoxy-1,10-phenanthroline (327 mg, 1.36 mmol). After bubbling nitrogen through the resulting solution for 30 min, the mixture was stirred at 90 degree for 10 h. It was allowed to cool down to room temperature and H2O (100 mL) was added. The aqueous layer was separated and extracted with ethyl acetate (2*200 mL). The combined organic layers was washed with brine (100 mL) and dried over sodium sulfate. The drying agent was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified on flash column eluting with PE/EA (15:1) to afford 102b (172 mg, 30%). LCMS: [M+H]+ 421. 1H NMR (500 MHz, CDCl3) delta 10.20 (s, 1H), 8.20 (s, 1H), 7.49-7.51 (m, 3H), 7.25 (m, 1H), 1.36 (s, 9H).

As the paragraph descriping shows that 1242156-59-7 is playing an increasingly important role.

Reference£º
Patent; GENENTECH, INC.; Crawford, James John; Ortwine, Daniel Fred; Wei, BinQing; Young, Wendy B.; US2013/116246; (2013); A1;,
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New learning discoveries about 253-52-1

As the paragraph descriping shows that 253-52-1 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.253-52-1,Phthalazine,as a common compound, the synthetic route is as follows.

Phthalazine (1) (91 mg, 0.70 mmol), 1,1-dicyanoalkene 2(0.70 mmol), and isocyanide 3 (0.70 mmol) were dissolvedin acetonitrile (1 ml). After that, distilled water(0.05?0.1 ml) was added to the reaction mixture up tovisible turbidity and stirred at 25?30¡ãC for 12?18 h. Thereaction mixture was evaporated to dryness and product 4was purified by crystallization from ethanol. 3-(tert-Butylamino)-2-phenylpyrrolo[2,1-a]phthalazine-1-carbonitrile (4a). Reaction time 18 h. Yield 204 mg(86percent), pale-yellow crystals, mp 173?174¡ãC. IR spectrum,nu, cm?1: 3385 (NH), 3065, 2861 (CH), 2226 (CN), 1604,1486, 764, 729 (Ar). 1H NMR spectrum, delta, ppm (J, Hz):8.90 (1H, s, H-6); 8.75 (1H, d, J = 8.0, H-10); 8.05?7.25(8H, m, H Ar); 4.12 (1H, br. s, NH); 0.99 (9H, s, 3CH3).13C NMR spectrum, delta, ppm: 146.1 (=N); 134.4 (?NH);131.4 ( Ar); 129.8 ( Ar); 129.5 ( Ar); 129.1 ( Ar);128.8 ( Ar); 128.0 ( Ar); 126.1 ( Ar); 125.9 ( Ar);124.7 ( Ar); 122.5 ( Ar); 120.0 ( Ar); 116.2 ( Ar);112.7 (CN); 100.2 ( Ar); 55.4 ((CH3)3); 31.4 (CH3).Mass spectrum, m/z (Irel, percent): 340 [M]+ (17), 314 (12), 284(100), 222 (13), 206 (10), 168 (18), 129 (12), 56 (89).Found, percent: C 77.79; H 6.10; N 16.51. 22H20N4. Calculated, percent: C 77.62; H 5.92; N 16.46.

As the paragraph descriping shows that 253-52-1 is playing an increasingly important role.

Reference£º
Article; Mironov, Maxim A.; Shulepov, Iliya D.; Kozhikhova, Ksenia V.; Ivantsova, Maria N.; Tokareva, Maria I.; Chemistry of Heterocyclic Compounds; vol. 53; 4; (2017); p. 430 – 433; Khim. Geterotsikl. Soedin.; vol. 53; 4; (2017); p. 430 – 433,4;,
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Some tips on 75884-70-7

75884-70-7 6-Bromophthalazin-1(2H)-one 11535918, aphthalazine compound, is more and more widely used in various.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.75884-70-7,6-Bromophthalazin-1(2H)-one,as a common compound, the synthetic route is as follows.

To a suspension of 6-bromophthalazine-l-(2H)-one (563 mg, 2.5 mmol) in DMF (25 mL) under an argon atmosphere was added sodium hydride (140 mg of 60% oil dispersion, 3.5 mmol) and the resulting mixture was allowed to stir at room temperature for 15 min. before addition of (2-(chloromethoxy)ethyl)trimethylsilane (0.53 mL, 3 mmol). The reaction mixture was stirred at room temperature overnight, then poured onto water and ether and extracted with ether (3X). The combined organic layer was washed with water, then brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was slurried in DCM and filtered. The solid was washed with DCM. The combined filtrate and wash was purified by chromatography to provide 6-bromo-2-((2-(trimethylsilyl)ethoxy)methyl)phthalazin-l(2H)-one (625 mg, 70% yield) as a white solid. NMR (300 MHz, Chloroform-^ delta 8.37 – 8.29 (m, 1H), 8.12 (s, 1H), 7.93 – 7.85 (m, 2H), 5.57 (s, 2H), 3.84 – 3.62 (m, 1H), 1.10 – 0.89 (m, 1H), 0.01 (s, 9H).

75884-70-7 6-Bromophthalazin-1(2H)-one 11535918, aphthalazine compound, is more and more widely used in various.

Reference£º
Patent; UNIVERSITY OF HAWAII; TURKSON, James; YUE, Peibin; TIUS, Marcus; BROTHERTON-PLEISS, Christine; LOPEZ TAPIA, Francisco, Javier; (420 pag.)WO2018/136935; (2018); A1;,
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Simple exploration of 1242156-59-7

1242156-59-7 6-(tert-Butyl)-8-fluorophthalazin-1(2H)-one 59473765, aphthalazine compound, is more and more widely used in various.

1242156-59-7, 6-(tert-Butyl)-8-fluorophthalazin-1(2H)-one is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a 100 mL round bottom flask series added compound 4-1 (1.77 g, 8.04 mmol), commercially available starting material 4-2 (1.40 g, 8.84 mmol) and cesium carbonate (1.90 g, 4.82 mmol). The flask was evacuated and back filled with nitrogen three times. Then ethoxytrimethylsilane (1.90 g, 16.07 mmol) and DMF (20 mL) were added to the reaction flask, and the resulting mixture was heated 62C. After 5 h stirring, the solution was allowed to cool down to ambient temperature and the reaction was quenched by addition 20 mL of water. The desired product started to precipitate from DMF and watermixture. The solid was collected by filtration after cooling down to 5C, and washed with water. The filter cake was dried under vacuum oven at 50C to afford crude compound 3 (2.88 g, yield:99.8%) as a light yellow solid which was used for next step without purification.

1242156-59-7 6-(tert-Butyl)-8-fluorophthalazin-1(2H)-one 59473765, aphthalazine compound, is more and more widely used in various.

Reference£º
Patent; CHEN, Yi; WO2015/50703; (2015); A1;,
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Analyzing the synthesis route of 119-39-1

The synthetic route of 119-39-1 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.119-39-1,Phthalazin-1(2H)-one,as a common compound, the synthetic route is as follows.

Example 1 Conventional Method of Preparation of Hydralazine Hydrochloride. A. Conventional Preparation of 1-Chlorophthalazine. One mole equivalent (10 g) of 1(2H)-phthalazinone and 7.7 mole equivalents (82.5 g, 50.1 mL) of phosphorus oxychloride were charged into a 100-mL, 3-necked flask fitted with a temperature probe and condenser. The slurry was stirred and heated to 70 C., and then the heat source was removed. The mixture was allowed to cool to room temperature, and then was poured in portions over 500 g of ice. After the initial addition of the reaction mixture, a violent exotherm was observed, and a portion of the solution spilled over the sides of the container. Ice quenching was completed with extreme caution but without further incident. Alternative workups were also examined. As a first alternative, after the reaction mixture reached room temperature, it was concentrated by heating at 45 C. under vacuum. The resulting yellow slurry was added in portions to 3 volumes of cold, deionized water. Once again, control of exothermic reactions that occurred during this quenching step was difficult. As a second alternative, after the reaction mixture reached room temperature, it was concentrated by heating at 45 C. under vacuum. To the resulting oily yellow paste was added 5 volumes of toluene, and the resulting biphasic solution was concentrated by heating at 45 C. under vacuum to remove the phosphorus oxychloride/toluene azeotrope. The process was repeated a second time. The resulting yellow paste solidified into an unworkable solid that was discarded. As a third alternative, after the reaction mixture reached room temperature, it was concentrated by heating at 45 C. under vacuum. To the resulting oily yellow paste was added 2 volumes of toluene, and the resulting biphasic solution was concentrated by heating at 45 C. under vacuum to remove the phosphorus oxychloride/toluene azeotrope. The process was repeated a second time, and then 2 volumes of tetrahydrofuran were added. The resulting slurry was stirred and cooled to 0 C. and then was filtered to isolate a light yellow solid. The filtrate was treated as described in the following paragraph. The aqueous mixture was rendered basic by the addition of 5 N sodium hydroxide solution. A light yellow precipitate formed. The solid was isolated by extraction into dichloromethane and concentration of the resulting extracts to dryness. A moist cake of 1-chlorophthalazine was thus obtained in yields that ranged from 80% to 440% of theoretical. If the moist cake was allowed to dry, or if this material was not used immediately, it darkened and underwent degradation to a mixture of the desired product, 1-chlorophthalazine, and multiple by-products. To prevent this loss and contamination, freshly obtained, moist chloro compound was used immediately.; Example 2 Novel Method for the Preparation of Hydralazine Hydrochloride. A. Novel Preparation of 1-Chlorophthalazine. One mole equivalent (250 g) of 1 (2H)-phthalazinone and 3.8 mole equivalents (775 g) of phosphorus oxychloride were charged into a 3-L, 3-necked flask fitted with a temperature probe and condenser. The slurry was stirred and heated to 80 C., maintained at that temperature for 30 minutes, and then the heat source was removed. Thin layer chromatographic analysis indicated that conversion to 1-chlorophthalazine was complete. The mixture was allowed to cool to room temperature, and 1.6 L of hexanes was added. The resulting slurry was stirred for several minutes, and the hexane layer was decanted. Addition of hexanes and decantation was repeated two more times. Then 1.6 L of tetrahydrofuran was added; as the solution was stirred, an off-white precipitate formed. The solid was isolated by filtration and washed with 250 mL of cold tetrahydrofuran to afford an 85-100% yield of 1-chlorophthalazine, the desired product, as an off-white powder that could be dried and characterized.;

The synthetic route of 119-39-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Nelson, Deanna J.; Barbeau, Donald L.; US2005/137198; (2005); A1;,
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Brief introduction of 119-39-1

The synthetic route of 119-39-1 has been constantly updated, and we look forward to future research findings.

119-39-1, Phthalazin-1(2H)-one is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A. Conventional Preparation of 1-Chlorophthalazine. One mole equivalent (10 g) of 1(2H)-phthalazinone and 7.7 mole equivalents (82.5 g, 50.1 mL) of phosphorus oxychloride were charged into a 100-mL, 3-necked flask fitted with a temperature probe and condenser. The slurry was stirred and heated to 70 C., and then the heat source was removed. The mixture was allowed to cool to room temperature, and then was poured in portions over 500 g of ice. After the initial addition of the reaction mixture, a violent exotherm was observed, and a portion of the solution spilled over the sides of the container. Ice quenching was completed with extreme caution but without further incident. Alternative workups were also examined. As a first alternative, after the reaction mixture reached room temperature, it was concentrated by heating at 45 C. under vacuum. The resulting yellow slurry was added in portions to 3 volumes of cold, deionized water. Once again, control of exothermic reactions that occurred during this quenching step was difficult. As a second alternative, after the reaction mixture reached room temperature, it was concentrated by heating at 45 C. under vacuum. To the resulting oily yellow paste was added 5 volumes of toluene, and the resulting biphasic solution was concentrated by heating at 45 C. under vacuum to remove the phosphorus oxychloridettoluene azeotrope. The process was repeated a second time. The resulting yellow paste solidified into an unworkable solid that was discarded. As a third alternative, after the reaction mixture reached room temperature, it was concentrated by heating at 45 C. under vacuum. To the resulting oily yellow paste was added 2 volumes of toluene, and the resulting biphasic solution was concentrated by heating at 45 C. under vacuum to remove the phosphorus oxychloride/toluene azeotrope. The process was repeated a second time, and then 2 volumes of tetrahydrofuran were added. The resulting slurry was stirred and cooled to 0 C. and then was filtered to isolate a light yellow solid. The filtrate was treated as described in the following paragraph. The aqueous mixture was rendered basic by the addition of 5 N sodium hydroxide solution. A light yellow precipitate formed. The solid was isolated by extraction into dichloromethane and concentration of the resulting extracts to dryness. A moist cake of 1-chlorophthalazine was thus obtained in yields that ranged from 80% to 440% of theoretical. If the moist cake was allowed to dry, or if this material was not used immediately, it darkened and underwent degradation to a mixture of the desired product, 1-chlorophthalazine, and multiple by-products. To prevent this loss and contamination, freshly obtained, moist chloro compound was used immediately.

The synthetic route of 119-39-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Nelson, Deanna J.; US2005/137397; (2005); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem