Month: September 2020

As a common heterocyclic compound, it belong phthalazine compound,Phthalazin-1(2H)-one,119-39-1,Molecular formula: C8H6N2O,mainly used in chemical industry, its synthesis route is as follows.,119-39-1

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.

With the synthetic route has been constantly updated, we look forward to future research findings about Phthalazin-1(2H)-one,belong phthalazine compound

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

As a common heterocyclic compound, it belongs to quinuclidine compound,Quinuclidine-4-carboxylic acid hydrochloride,40117-63-3,Molecular formula: C8H14ClNO202,mainly used in chemical industry, its synthesis route is as follows.,253-52-1

A. A solution of phthalazine (2.5 g, 19.2 mmol) in concentrated sulfuric acid (30 mL) is treated slowly with potassium nitrate (2 g, 19.2 mmol). After 18 h the solution is cooled. Water (30 mL) is added. The solution is basified using 10 M NaOH to pH 13 (litmus). The solution is cooled for 18 h, filtered to give 5-nitro-phthalazine (0.93 g).

With the complex challenges of chemical substances, we look forward to future research findings about Phthalazine,belong phthalazine compound

Reference£º
Patent; Calvo, Raul R.; Cheung, Wing S.; Player, Mark R.; US2006/116368; (2006); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

It is a common heterocyclic compound, the phthalazine compound, Phthalazine, cas is 253-52-1 its synthesis route is as follows.,253-52-1

To a stirred solution of furan (1.20 g,17.6 mmol) in dry THF (20 mL) was added dropwise n-butyllithium (2.5 M in hexanes, 7.30 mL,18.3 mmol) over a period of 30 min at ?78 ¡ãC. The solution was warmed to ?25 ¡ãC, and stirring wascontinued at this temperature for 30 min. The reaction mixture was cooled back to ?78 ¡ãC, and asolution of 1 (2.00 g, 15.3 mmol) in dry THF (20 mL) was added dropwise over 30 min. The reaction mixture was stirred at this temperature for 2 h. The mixture was poured into saturated NH4Cl(100 mL) and extracted with ethyl acetate (3 ¡Á 50 mL). The combined organic extracts were thenwashed with saturated NaCl (50 mL), dried (MgSO4), filtered, and concentrated under vacuum toafford 3f as a light brown oil. The crude product 3f was dissolved in DCM (30 mL), and triethylamine(2.37 g, 3.26 mL, 23.4 mmol) was added, followed by dropwise addition of acryloyl chloride (1.59 g,1.43 mL, 17.6 mmol) at 0 ¡ãC. The reaction mixture was stirred at 0 ¡ãC for 2 h. The reaction was thenquenched with saturated NaCl (25 mL), and the organic layer was separated. The aqueous layer wasextracted with DCM (2 ¡Á 30 mL), and the combined organic extracts were washed with saturated NaCl(50 mL), dried (MgSO4), filtered, and concentrated to afford the crude product. The product waspurified on a silica gel column eluted with hexanes?EtOAc (7:3) to afford 4f (2.66 g, 60percent) as a yellowliquid.

With the complex challenges of chemical substances, we look forward to future research findings about Phthalazine

Reference£º
Article; Nammalwar, Baskar; Muddala, N.Prasad; Bourne, Christina R.; Henry, Mary; Bourne, Philip C.; Bunce, Richard A.; Barrow, Esther W.; Berlin, K.Darrell; Barrow, William W.; Molecules; vol. 19; 3; (2014); p. 3231 – 3246;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

253-52-1, Phthalazine is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 13 Preparation of 4-(4-Acetylaminophenyl)-1,2-Dihydro-6-Methylthiophthalazine (15) To a solution of the phthalazine 7 (130 mg, 0.42 mmol) in acetic acid (7 mL) was added NaBH3CN in portions. After stirring for 15 min, water was added. The aqueous phase was neutralized by NaHCO3, and then extracted with DCM. The combined organic phase was dried over Na2SO4. Removal of the solvent afforded the product (97 mg, 74percent) which can be used directly for next step.

253-52-1, The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Pei, Xue-Feng; Li, Baoqing; Maccecchini, Maria-Luisa; US2002/6925; (2002); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

Phthalazine, cas is 253-52-1, it is a common heterocyclic compound, the phthalazine compound, its synthesis route is as follows.,253-52-1

Specific preparation methods are: no special protection, clean air to a single-necked flask were added sequentially magneton, phthalazine(52mg, 0.4mmol), was added sodium iodide (18mg, 30molpercent), 70percent of the mass fraction of the water phase of t-butyl hydroperoxide(152mg, 1.2mmol), then add toluene (728.8mg, 8mmol), toluene as both reactant and as a solvent, the reaction at 150 1Hours TLC showed the starting material is completely consumed phthalazine. Heating was stopped to quench the reaction. Without extraction, direct wetLoading, 200-300 mesh silica gel column chromatography, a mixed solvent of ethyl acetate and petroleum ether (1: 4) rinse. Separated structure of formula IXaFormula compound 84.0mg, 89percent yield;

With the rapid development of chemical substances, we look forward to future research findings about Phthalazine

Reference£º
Patent; Xiangtan University; Yang, Luo; Luo, Wenkun; (17 pag.)CN105503724; (2016); A;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

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

To a round bottom flask containing DMF (30 mL) under an atmosphere of nitrogen was added, phthalazone (500 mg, 3.42 mmol), anhydrous potassium carbonate (708 mg, 5.12 mmol) and allyl bromide (442 pL, 5.12 mmol). The reaction was stirred overnight at room temperature before the solvent was removed in vacuo and the crude material purified directly via flash column chromatography using n -pentane: EtOAc (3:1) affording 2-allylphthalazin- 1 (2/7)-onc as a brown oil (222 mg, 1.20 mmol, 35%) NMR (400 MHz, CDCb) d = 8.42 (ddd, J = 7.5, 1.7, 0.7 Hz, 1H), 8.17 (d, J = 0.8 Hz, 1H), 7.83 – 7.72 (m, 2H), 7.71 – 7.67 (m, 1H), 6.04 (ddt, / = 17.2, 10.3, 5.9 Hz, 1H), 5.30 – 5.22 (m, 2H), 4.85 (dt, J = 5.9, 1.5 Hz, 2H); 13C NMR (100 MHz, CDCb) d = 159.2, 138.1, 133.1, 132.5, 131.7, 129.7, 128.0, 126.8, 126.0, 118.0, 53.5. Data is in accordance with literature values (Nezhawy, A.O.H., Gaballah, S.T. & Radwan, M.A.A. Studying the reactivity of (phthalazin-l(2H)-on-2-yl)methyl trichloroacetimidate towards different C- and O-nucleophiles. Tetrahedron Letters 50, 6646-6650, 2009)., 119-39-1

119-39-1 Phthalazin-1(2H)-one 8394, aphthalazine compound, is more and more widely used in various fields.

Reference£º
Patent; OXFORD UNIVERSITY INNOVATION LIMITED; GOUVERNEUR, Veronique; CORNELISSEN, Bart; WILSON, Thomas Charles; (152 pag.)WO2019/186135; (2019); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

A common heterocyclic compound, the phthalazine compound, name is Phthalazin-1(2H)-one,cas is 119-39-1, mainly used in chemical industry, its synthesis route is as follows.,119-39-1

261.3 mg of acetic anhydride copper (II) and Molecular Sieve 4A (79.1 mg) were added to 80.7 mg of the resin obtained in Process 4. 400.0 mg of 1(2H)-phthalazinone and 984 mul of diisopropylethylamine in a solution of NMP (4 ml) were further added therein and stirred at 50C for 23 hours. After removing the reaction solution, the resin was washed with DMF, water, ethanol and DCM three times each and dried under reduced pressure.

As the rapid development of chemical substances, we look forward to future research findings about 119-39-1

Reference£º
Patent; Ajinomoto Co., Inc.; EP1454898; (2004); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

253-52-1, Phthalazine is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: 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.

253-52-1, 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;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

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 6 Preparation of 1-Chlorophthalazine Hydrochloride A 3-neck 2 L round-bottomed flask was charged with 584 mL of phosphorous oxychloride (306 g, 2 mol. eq.) and cooled to about 0 to 5 C. To this was added 73 g of powdered phthalazinone (0.5 mol eq.). The reaction mass appeared as a suspension and was heated to about 60 C. with stirring. The progress of the reaction was monitored by HPLC. While the reaction mixture was maintained at approximately 50 C., about 65% of the phosphorous oxychloride was distilled out under vacuum. The concentrated reaction mixture was cooled to room temperature, about 375 mL of ethyl acetate was added, and then the mixture was purged with HCl gas for about 30 min.; thereafter, the mixture was cooled to a temperature of 0 to 5 C. and stirred for about one hour. The resulting pale yellow material was filtered and washed with 150 mL of cold ethyl acetate. The isolated material was 1-chlorophthalazine hydrochloride, which was dried under vacuum for about 3 hrs at 30 C. Yield=65%; purity=99%;, 119-39-1

119-39-1 Phthalazin-1(2H)-one 8394, aphthalazine compound, is more and more widely used in various fields.

Reference£º
Patent; Navinta LLC; US2007/129546; (2007); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

253-52-1, Phthalazine is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A solution of 3.0g (23.3mmol) of phthalazine in 20mL of concentrated sulfuric acid was brought to 100C. To the phthalazine solution was added portion-wise 18.8g (186mmol) of potassium nitrate over 1-h time period. After 72h at 100C, the solution was cooled to room temperature, poured over ice, and neutralized with ammonium hydroxide to produce a yellow-tan precipitate. The precipitate was collected and dried to afford 2.3g (56%) of the 5-nitrophthalazine intermediate as a light yellow solid. 1H NMR (400MHz, DMSO-d6) delta: 10.2 (s, 1 H), 9.98 (s, 1 H), 8.84 (d, J=7.4Hz, 1H), 8.59 (d, J=7.6Hz, 1H), 8.20 (dd, J=7.4, 14.9Hz, 1H). 13C NMR (100.17MHz, DMSO-d6) delta: 152.1, 146.3, 141.0, 133.2, 131.8, 130.0, 127.4, 118.7.

253-52-1, 253-52-1 Phthalazine 9207, aphthalazine compound, is more and more widely used in various fields.

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;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem