Month: September 2020

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

Phthalazin-1(2H)-one (7 mmol) and POCl3 (56 mmol) were charged into a 100-mL, 3-necked flask and heated at 75C for 30 min. After being cooled to room temperature, the mixture was poured into ice water and then added additional 10% NaOH until the pH of the solution is 7.5. The solid was isolated by filtration and washed with 2 ml iced water. The resulting solid was dissolved in EtOH (6 ml), to which 50% hydrazine hydrate (3 ml) was added. After stirring at 60-70C for 2h, the pH value of the mixture was adjusted to 3 with 15% hydrochloric acid. Then the mixture was cooled to 0-5C. The solid was isolated by filtration, washed with iced EtOH (2 ml), and dried, giving the desired product (894 mg, 65% yield).

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

Reference£º
Article; Liu, Bin; Zhang, Chunlei; Zhou, Xigeng; Tetrahedron; vol. 72; 50; (2016); p. 8282 – 8286;,
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

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.

With the rapid development of chemical substances, we look forward to future research findings about 253-52-1

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

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

A mixture of the commercially available phthalazin-l(2//)-one (5.0 g, 34.0 mmol) and phosphorus oxychloride (POCh) (25 mL) was heated with stirring at l00C for 2 h. After cooling to room temperature, the excess POCI3 was completely distilled out under reduced pressure. The residue was triturated with toluene (2 x 25 mL) and followed with THF (100 mL), and the solid product was collected by filtration and washed with THF. The product was then dissolved in DCM, washed with saturated aqueous NaHC03 solution, dried over sodium sulfate and evaporated under reduced pressure to give 1- chlorophthalazine. Yield 4.6 g (82%); mp 119-121 C (lit.33 mp 132-134 C). (0220) [0134] NMR (DMSO-^e) d 8.20 (2H, t, J = 7.2 Hz, ArH), 8.33 (2H, t, J = 7.6 Hz, ArH), 9.73 (1H, s, ArH). (0221) [0135] 13C NMR (DMSO-?) d 126.1, 128.4, 128.7, 155.3. HRMS [ESL]: calculated for C8H5ClN2, 165.0220 [M+H]+, found 165.0212.

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

Reference£º
Patent; ACADEMIA SINICA; SU, Tsann-long; LEE, Te-chang; CHEN, Tai-lin; (92 pag.)WO2019/99755; (2019); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

75884-70-7, 6-Bromophthalazin-1(2H)-one is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,75884-70-7

6-bromopyridazine-1(2H)-one (0.80 g, 3.55 mmol), A solution of cesium carbonate (2.89 g, 8.86 mmol) and 2-chloromethyloxazole (0.50 g, 4.25 mmol) in N,N-dimethylformamide (10 mL) was stirred at 50 C for 5 h. The reaction system was cooled to room temperature, poured into water, and the solid was collected by filtration. Wash the filter cake with water and petroleum ether, respectively. Drying under reduced pressure gave Compound 3.1 (0.84 g, yield: 78%) as a yellow solid.

As the paragraph descriping shows that 75884-70-7 is playing an increasingly important role.

Reference£º
Patent; Shanghai Dinuo Pharmaceutical Technology Co., Ltd.; Gao Daxin; Yang Heping; Chen Shoujun; Gao Yaqiao; Wang Longsheng; (32 pag.)CN109721597; (2019); A;,
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

General procedure: N-heteroarene (1 mmoL, 80 mg), alpha-keto acid (3 mmol), Formic acid (1 mmol, 38 muL), ammonium persulfate (3 mmoL, 685 mg), ferrous sulfate heptahydrate (0.08 mmoL, 22 mg) and 20 mL of mixed solvent (DCM: H2O = 3: 1) , 0.1 mL DMSO was added into a 25 mL round-bottomed flask. The mixture was stirred at 40 oC until TLC analysis indicating that the reaction was complete (witnessed by the disappearance of the N-heteroarene). After separation of organic phase, the residue was neutralized by 0.1 M sodium hydroxide solution, then extracted with DCM (3¡Á20 mL), combined the organic phases, dried over Na2SO4, and concentrated in vacuo. The residue was N-heteroarene (1 mmoL, 80 mg), alpha-keto acid (3 mmol), Formic acid (1 mmol, 38 muL), ammonium persulfate (3 mmoL, 685 mg), ferrous sulfate heptahydrate (0.08 mmoL, 22 mg) and 20 mL of mixed solvent (DCM: H2O = 3: 1) , 0.1 mL DMSO was added into a 25 mL round-bottomed flask. The mixture was stirred at 40 oC until TLC analysis indicating that the reaction was complete (witnessed by the disappearance of the N-heteroarene). After separation of organic phase, the residue was neutralized by 0.1 M sodium hydroxide solution, then extracted with DCM (3¡Á20 mL), combined the organic phases, dried over Na2SO4, and concentrated in vacuo. The residue was purified by column chromatography on silica gel using a mixture of petroleum ether/EtOAc (v : v = 20 : 1) as eluent to afford the desired pure product.

With the rapid development of chemical substances, we look forward to future research findings about 253-52-1

Reference£º
Article; Wang, Xiu-Zhi; Zeng, Cheng-Chu; Tetrahedron; vol. 75; 10; (2019); p. 1425 – 1430;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

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

General procedure: Method A A mixture of 4-bromophthalazin-1(2H)-one (3) (2.22mmol), potassium carbonate (6.66mmol) in dry acetone (20mL) was heated to boiling for 30 min and next methyl iodide (3.33mmol) was added. The reaction mixture was heated and stirred under reflux for 8h. Method B A mixture phthalazin-1(2H)-one (2) (3.42mmol), caesium carbonate (4.11 mmol) in dry acetone (20 mL) was charged to PTFE tubes, sealed in ceramic cases and placed in the rotor. The reaction mixture was heated to 55C, held for 0.5 h at 55C and then cooled to 25C. In the next step the methyl iodide (0.23mL, 3.77mmol) was added and the reaction was continued at 55C for 3.5h. After cooling to room temperature the separated solid was collected by filtration and washed with acetone (5mL). The filtrate was concentrated under reduced pressure and then the crude product was purified by flash chromatography.

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

Reference£º
Article; Malinowski, Zbigniew; Fornal, Emilia; Sieroci?ska, Beata; Czeczko, Renata; Nowak, Monika; Tetrahedron; vol. 72; 49; (2016); p. 7942 – 7951;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

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

General procedure: Method A The Mitsunobu reaction was carried out under argon. Diethyl azodicarboxylate (1.03 mmol, solution in toluene c?40%) was slowly added to a stirred solution of triphenylphosphine (1.03 mmol) in dry THF (10mL) at the temperature between -10C and -5C. Then a solution of phthalazinone 2 (0.684 mmol) in THF (10 mL) was added dropwise. The whole lot was mixed for 15 min at this temperature and next the appropriate alcohol (0.753 mmol) in THF (5 mL) was added at -10 to -5C. The mixture was stirred during 2 h at this conditions, after, which time the reaction mixture was warmed to ambient temperature and stirred in this conditions for 24h. All volatile materials were removed under reduced pressure, ethyl ether (5 mL) was added to the residue, and the whole lot was stirred for 0.5 h at an ambient temperature. The separate white solid was collected by flirtation and washed with ether, and the filtrate was evaporated to dryness. The product was separated and purified by flash chromatography. Method B The Mitsunobu reaction was carried out under argon. To a round bottom flask were added phthalazinone 2 or 3 (1.78 mmol), alcohol (2.67 mmol), triphenylphosphine (2.67 mmol) and THF (40 mL). Then, the solution was cooled to the temperature -20C for 15 min and diethyl azodicarboxylate (2.67mmol, solution in toluene c?40%) was added dropwise to the solution. The reaction was stirred at -20C for 1h, and then the cold bath allowed to slowly warm to an ambient temperature and stirred in this conditions for 24h. All volatile materials were removed under reduced pressure, diethyl ether (15 mL) was added to the residue, and the whole lot was stirred for 0.5 h at an ambient temperature. The separate white solid was collected by flirtation and washed with ether, and the filtrate was evaporated to dryness. The product was separated and purified by flash chromatography.

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

Reference£º
Article; Malinowski, Zbigniew; Fornal, Emilia; Sieroci?ska, Beata; Czeczko, Renata; Nowak, Monika; Tetrahedron; vol. 72; 49; (2016); p. 7942 – 7951;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

1021298-68-9, 2-Fluoro-5-((4-oxo-3,4-dihydrophthalazin-1-yl)methyl)benzonitrile is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Add Compound III 25.82 g to the reaction flask.Purified water 100ml,Stir at room temperature,Then add 22.4M sodium hydroxide 92.4ml,The mixture temperature was heated to 100 C,Stir 12h, cool to room temperature, filter, wash,The combined filtrate was acidified with 46.2 ml of 2M diluted hydrochloric acid for 30 min,Then, 500 ml of methanol, 18.70 g of triethylamine, and 14.25 g of 1-cyclopropanecarbonylpiperazine are added successively.At a reaction temperature of 20-25C, the reaction is stirred for 10 hours. After the reaction is completed, it is cooled to 0C and filtered.38.66 g of solids were obtained with a yield of 96.2% and a purity of 99.89%. The refining of olaparib (I)30g of crude oleapani was placed in a dissolving tank81.82 ml of isopropanol and 818.2 ml of acetone were added and the temperature was controlled at 45-50C.Stir and dissolve. After the crude product is completely dissolved, add charcoal to decolorize it for 30 minutes.The decolorization reaction was followed by hot filtration and the filtrate was stirred at room temperature for crystallization.Then cool down to 0 ~ 10 C for 4 hours, filter, and wash with acetone,Filtration, drying, that is, olaparib 28.35g,The yield was 94.5%, the purity was 99.99%, the mononuclear 0.05%, and the total heterologous 0.11%., 1021298-68-9

The synthetic route of 1021298-68-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Shandong Yuxin Pharmaceutical Co., Ltd.; Liu Zhenteng; Chen Yu; Sun Heng; Wang Chunyan; (6 pag.)CN108101852; (2018); A;,
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

General procedure: A solution of sodium azide (0.085 g, 1.3 mmol) in water (10 ml) was slowly added to the methanolic solution (15 ml) of Cd(NO3)24H2O (0.2 g, 0.65 mmol) and quinazoline (0.17 g, 1.30 mmol) and stirred at room temperature for 12 h. Light yellow crystalline precipitate of [Cd(Qnz)2(N3)2]n was collected in 70percent yield. The crystals suitable for X-ray structure determination were obtained by slow recrystallization from methanol

With the rapid development of chemical substances, we look forward to future research findings about 253-52-1

Reference£º
Article; Machura; Nawrot; Kruszynski; Dulski; Polyhedron; vol. 54; (2013); p. 272 – 284;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem