Tag: M.W:100-200

As a common heterocyclic compound, it belongs to phthalazine compound, name is Phthalazin-1(2H)-one, and cas is 119-39-1, its synthesis route is as follows.,119-39-1

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.;

With the complex challenges of chemical substances, we look forward to future research findings about 119-39-1,belong phthalazine compound

Reference£º
Patent; Nelson, Deanna J.; Barbeau, Donald L.; US2005/137198; (2005); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

Name is Phthalazin-1(2H)-one, as a common heterocyclic compound, it belongs to phthalazine compound, and cas is 119-39-1, its synthesis route is as follows.

To a round bottom flask containing THF (10 mL) under an atmosphere of nitrogen was added, phthalazone (500 mg, 3.41 mmol), di-/c/ -butyl dicarbonate (1.11 g, 5.12 mmol) and DMAP (620 mg, 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 -pentane: EtOAc (5: 1) tert- Butyl 1 -oxophthalazine-2( i H)- carboxylate as a white solid (765 mg, 3.11 mmol, 91%). 3H NMR (400 MHz, CDCb) d = 8.43 (dd, 7 = 7.9, 1.3 Hz, 1H), 7.83 (td, 7 = 7.5, 1.4 Hz, 1H), 7.77 (td, 7 = 7.6, 1.3 Hz, 1H), 7.68 (dd, 7 = 7.5, 1.3 Hz, 1H), 1.66 (s, 9H);13C NMR (100 MHz, CDCb) d = 158.3, 150.9, 138.9, 134.2, 132.3, 129.2, 128.7, 127.5, 126.4, 85.9, 27.8 (3C); IR (v, cm4): 2980, 1720, 1641, 1470, 1325, 1130; HRMS (ESI) for C13H14N2O3 (0556) [M+H]+ requires 247.1012 found 247.1015; Mp: 81 – 83C

119-39-1, In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles.,119-39-1 ,Phthalazin-1(2H)-one, other downstream synthetic routes, hurry up and to see

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

253-52-1, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. Phthalazine, cas is 253-52-1,the phthalazine compound, it is a common compound, a new synthetic route is introduced below.

Example 1A1,2-phenylenedimethanamine[0168]Phthalazine (21.5 g, 0.165 mol), 10percent palladium on carbon (2 g), and methanol (125 mL) were combined in a pressure bottle and shaken at room temperature under 60 psi of hydrogen for 5 days. Raney-nickel? slurry (6.42 g) and 10percent palladium on carbon (0.50 g) were added, and the mixture was shaken at 50¡ã C. under 60 psi of hydrogen for 16 hours. The mixture was filtered through a nylon membrane and concentrated to give the titled compound: 1H NMR (300 MHz, DMSO-d6) delta ppm 7.32 (dd, J=5.4, 3.5 Hz, 2H), 7.17 (dd, J=5.6, 3.4 Hz, 2H), 3.74 (s, 4H); MS (DCI/NH3) m/z 137 (M+H)+.

The chemical industry reduces the impact on the environment during synthesis,253-52-1,Phthalazine,I believe this compound will play a more active role in future production and life.

Reference£º
Patent; AbbVie Inc.; Cowart, Marlon D.; Liu, Huaqing; Altenbach, Robert; US2013/40940; (2013); 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.

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, In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles.,253-52-1 ,Phthalazine, other downstream synthetic routes, hurry up and to see

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

253-52-1, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. Phthalazine, cas is 253-52-1,the phthalazine compound, it is a common compound, a new synthetic route is introduced below.

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.

The chemical industry reduces the impact on the environment during synthesis,253-52-1,Phthalazine,I believe this compound will play a more active role in future production and life.

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

Name is Phthalazin-1(2H)-one, as a common heterocyclic compound, it belongs to phthalazine compound, and cas is 119-39-1, its synthesis route is as follows.

2H-phthalazin-1-one (150 mmol), (3,4-dihydroisoquinolin-2(1H)-carboxylic acid tert-butyl ester-5-yl)-carbamic acid o-chlorophenyl ester (195 mmol) were placed in a reaction flask, then DMF100 ml was added and the reaction was carried out at 55 C overnight. The reaction was stopped, added 300 ml of ethyl acetate, 200ml of dichloromethane, and extracted. The organic phase was separated, and the aqueous phase was extracted with dichloromethane (3*50 ml). The organic phase was combined, dried over anhydrous sodium sulfate, and Purification by column chromatography gave the title compound.

119-39-1, In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles.,119-39-1 ,Phthalazin-1(2H)-one, other downstream synthetic routes, hurry up and to see

Reference£º
Patent; Nanjing Advanced Biological Materials And Process Equipment Institute Co., Ltd.; Guo Chengjie; (16 pag.)CN109336863; (2019); A;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

Name is Phthalazin-1(2H)-one, as a common heterocyclic compound, it belongs to phthalazine compound, and cas is 119-39-1, its synthesis route is as follows.

EXAMPLE 1 (COMPARATIVE) Preparation of 1-Chlorophthalazine According to the process disclosed in U.S. Pat. Pub. 20050137397, the disclosure of which is incorporated herein by reference, 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. The mixture was allowed to cool to room temperature and 1.6 L of hexane were added. The resulting slurry was stirred for about 30 minutes, allowed to settle, and the hexane layer was decanted; the addition of hexane and decantation was repeated three times. Then 1.6 L of tetrahydrofuran was added to the slurry and a yellow precipitate formed. The yellow solid (reported in the ‘397 application as an off white solid) was isolated by filtration and then washed with 250 mL of cold tetrahydrofuran to afford a 50% yield (reported yield in the ‘397 application is 85 to 100%) of 1-chlorophthalazine.

119-39-1, In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles.,119-39-1 ,Phthalazin-1(2H)-one, other downstream synthetic routes, hurry up and to see

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

It is a common heterocyclic compound, the phthalazine compound, Phthalazin-1(2H)-one, cas is 119-39-1 its synthesis route is as follows.,119-39-1

To a round bottom flask containing THF (10 mL) under an atmosphere of nitrogen was added, phthalazone (500 mg, 3.41 mmol), di-/c/ -butyl dicarbonate (1.11 g, 5.12 mmol) and DMAP (620 mg, 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 -pentane: EtOAc (5: 1) tert- Butyl 1 -oxophthalazine-2( i H)- carboxylate as a white solid (765 mg, 3.11 mmol, 91%). 3H NMR (400 MHz, CDCb) d = 8.43 (dd, 7 = 7.9, 1.3 Hz, 1H), 7.83 (td, 7 = 7.5, 1.4 Hz, 1H), 7.77 (td, 7 = 7.6, 1.3 Hz, 1H), 7.68 (dd, 7 = 7.5, 1.3 Hz, 1H), 1.66 (s, 9H);13C NMR (100 MHz, CDCb) d = 158.3, 150.9, 138.9, 134.2, 132.3, 129.2, 128.7, 127.5, 126.4, 85.9, 27.8 (3C); IR (v, cm4): 2980, 1720, 1641, 1470, 1325, 1130; HRMS (ESI) for C13H14N2O3 (0556) [M+H]+ requires 247.1012 found 247.1015; Mp: 81 – 83C

With the complex challenges of chemical substances, we look forward to future research findings about Phthalazin-1(2H)-one

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

It is a common heterocyclic compound, the phthalazine compound, Phthalazin-1(2H)-one, cas is 119-39-1 its synthesis route is as follows.,119-39-1

To a round bottom flask containing THF (10 mL) under an atmosphere of nitrogen was added, phthalazone (500 mg, 3.41 mmol), di-/c/ -butyl dicarbonate (1.11 g, 5.12 mmol) and DMAP (620 mg, 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 -pentane: EtOAc (5: 1) tert- Butyl 1 -oxophthalazine-2( i H)- carboxylate as a white solid (765 mg, 3.11 mmol, 91%). 3H NMR (400 MHz, CDCb) d = 8.43 (dd, 7 = 7.9, 1.3 Hz, 1H), 7.83 (td, 7 = 7.5, 1.4 Hz, 1H), 7.77 (td, 7 = 7.6, 1.3 Hz, 1H), 7.68 (dd, 7 = 7.5, 1.3 Hz, 1H), 1.66 (s, 9H);13C NMR (100 MHz, CDCb) d = 158.3, 150.9, 138.9, 134.2, 132.3, 129.2, 128.7, 127.5, 126.4, 85.9, 27.8 (3C); IR (v, cm4): 2980, 1720, 1641, 1470, 1325, 1130; HRMS (ESI) for C13H14N2O3 (0556) [M+H]+ requires 247.1012 found 247.1015; Mp: 81 – 83C

With the complex challenges of chemical substances, we look forward to future research findings about Phthalazin-1(2H)-one

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

89898-86-2, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 5-Nitrophthalazine, cas is 89898-86-2,the phthalazine compound, it is a common compound, a new synthetic route is introduced below.

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.

The chemical industry reduces the impact on the environment during synthesis,89898-86-2,5-Nitrophthalazine,I believe this compound will play a more active role in future production and life.

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