Month: August 2020

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) (0.78 g, 2.13 mmol) was added to a 25 ml three-necked flask.Dichloromethane (6.5 ml) and triethylamine (0.52 g, 5.14 mmol) were added, and the mixture was stirred and cooled to 1-10 C.Further, 2-butenyl chloride (268 mg, 2.56 mmol) was added dropwise, and the mixture was warmed to room temperature and stirred for 1 hour.TLC showed the reaction was complete; the reaction mixture was directly concentrated to dryness, and the residue was mixed with water and then stirred for 1 hour and then filtered.Obtained as an off-white solid.The yield was 37%.

As the paragraph descriping shows that 763111-47-3 is playing an increasingly important role.

Reference£º
Patent; Shanghai Bobang Pharmaceutical Technology Co., Ltd.; Gao Heyong; Liu Zhende; Zhang Wensheng; (28 pag.)CN108383798; (2018); A;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.152265-57-1,7-Bromophthalazin-1(2H)-one,as a common compound, the synthetic route is as follows.

A mixture of compound 50-d (600mg, 2.67mmol) and POCl3 (8mL) was heated to reflux for 1.5h, cooled toroom temperature and concentrated under reduced pressure. The residue was dissolved in DCM (40mL), washed inturn with saturated sodium bicarbonate (40mL) and saturated brine (10mL), dried over anhydrous sodium sulfate, filteredand concentrated under reduced pressure. The residue was purified by silica column chromatography (PE:EA = 3:1) togive compound 50-c (500mg, yield 75%). LC-MS (ESI): m/z = 243 [M+H]+.

152265-57-1 7-Bromophthalazin-1(2H)-one 22265317, aphthalazine compound, is more and more widely used in various.

Reference£º
Patent; Shanghai Yingli Pharmaceutical Co. Ltd.; XU, Zusheng; ZHANG, Nong; SUN, Qingrui; WU, Tianzhi; (104 pag.)EP3275867; (2018); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

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

example 2 B (1 eq) dissolved in anhydrous second grade nitrile, then adding to bromine methyl cinnamic acid methyl ester (1 eq) and DIEA (2 eq), under the protection of nitrogen reaction at room temperature 2 hours, the reaction produces a large amount of white precipitate. Slightly static delayed filtering and washing the filter cake to a small amount of acetonitrile, the title compound obtained (white solid, yield 64%).

763111-47-3 4-(4-Fluoro-3-(piperazine-1-carbonyl)benzyl)phthalazin-1(2H)-one 11726399, aphthalazine compound, is more and more widely used in various.

Reference£º
Patent; Graduate School at Shenzhen, Tsinghua University; Jiang Yuyang; Yuan Zigao; Gao Chunmei; Chen Shaopeng; (23 pag.)CN106946792; (2017); A;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

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

Step 3: A oven dried flask was charged with 1-(2-formyl-3-iodo-phenyl)-3-iodo-1H-pyrazole-4-carbonitrile (1.703 g, 3.79 mmol), 6-tert-butyl-8-fluorophthalazin-1(2H)-one [prepared according to US2010/0222325] (919 mg, 4.17 mmol) and sodium bicarbonate (637 mg, 7.59 mmol) and taken up in dry dimethyl sulfoxide (30 ml). The mixture was degassed with argon in a sonication bath. Copper iodide (722 mg, 3.79 mmol) was added and the material was again degassed thoroughly. With sonication the mixture was heated to 60 C. for 2.5 hours and left at ambient overnight. Additional copper iodide (360 mg) was added and the material was heated for 4 hours at 60 C. under sonication. The flask was cooled to ambient and methylene chloride (40 ml) and water (40 ml) were added, with vigorous stirring. After 5 minutes the material was filtered through a plug of celite, rinsing well with a solution of 1% methanol in methylene chloride. The filtrate was transferred to a separatory funnel and the organic phase was collected. This was shaken with a 50% diluted brine solution (60 ml, some ragging). The methylene chloride phase was collected and the aqueous phases were back extracted with methylene chloride (note: some ragging observed. It helps to use larger volumes of organic and aqueous solutions on back extraction). The combined organic phase was dried with magnesium sulfate, filtered and stripped. The remainder was taken up in methylene chloride and purified through Analogix flash column chromatography eluting first with 100% dichloromethane (hold for 5 minutes) and then switch to a gradient of 1% to 3% methanol in dichloromethane (25 g silica gel) providing the desired 1-[3-(6-tert-butyl-8-fluoro-1-oxo-1H-phthalazin-2-yl)-2-formyl-phenyl]-3-iodo-1H-pyrazole-4-carbonitrile as a light brown powder (1.2 g). LC/MS calc’d for C23H17FIN5O2 (m/e) 541.32, obs’d 542 (M+H, ES+).

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; Billedeau, Roland Joseph; Kondru, Rama K.; Lopez-Tapia, Francisco Javier; Lou, Yan; Owens, Timothy D.; Qian, Yimin; So, Sung-Sau; Thakkar, Kshitij C.; Wanner, Jutta; US2012/295885; (2012); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.103119-78-4,5-Bromophthalazine,as a common compound, the synthetic route is as follows.

Methyl phthalazine-5-carboxylate. To a 140 mL pressure flask was added 5-bromophthalazine (3.5 g, 17 mmol), palladium (II) acetate (0.98 g, 4.4 mmol), triphenylphosphine (1.3 g, 5.0 mmol), potassium acetate (2.1 g, 21 mmol), MeOH (20 mL) and DMF (20 mL). The flask was sealed and purged with CO (3 x). The flask was charged with CO to 40 PSI and stirred at 100¡ãC 15 hours. The suspension was filtered through Celite, the cake was washed with MeOH, and the filtrate was concentrated. The residue was taken up in DCM and washed with saturated sodium bicarbonate (2 x), saturated sodium chloride (2 x) and water (2 x). The organic layer was dried over sodium sulfate, filtered and concentrated in vacuo. The residue was adsorbed on to a plug of silica gel and purified by chromatography through a Redi-Sep pre-packed silica gel column, eluting with a gradient of EtOAc in hexane to provide methyl phthalazine-5- carboxylate (1.0 g, 32 percent). LCMS (M+H) 189.2 calc. for C10H9N2O2 189.1, 1H NMR (400 MHz, CDCl3): delta ppm 4.05 (s, 3H) 8.06 (d, J=8.41 Hz, 1H) 8.51-8.56 (m, 1H) 8.71 (d, 1H) 9.64 (s, 2H).

103119-78-4 5-Bromophthalazine 13649370, aphthalazine compound, is more and more widely used in various.

Reference£º
Patent; AMGEN INC.; WO2009/11871; (2009); A2;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

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

In a 1 L round-bottomed flask, 6-tert-butyl-8-fluorophthalazin-1(2H)-one (5.6 g, 25.4 mmol, Eq: 1.00) was combined with THF (300 ml) to give a colorless solution. Sodium hydride (1.12 g, 28.0 mmol, Eq: 1.1) was added. The reaction mixture was stirred at ambient temperature for 10 min 2-Fluoro-4-iodonicotinaldehyde (7.02 g, 28.0 mmol, Eq: 1.1) was added and the reaction mixture was stirred at ambient temperature for 1 h. The reaction was complete as determined by LCMS analysis. The reaction mixture was quenched with saturated NH4Cl. The reaction mixture was poured into 200 mL H2O and extracted 3X with CH2Cl2. The organic layers were washed with brine, then dried over Na2SO4 and concentrated in vacuo. The resultant bright yellow solid was transferred into a filter funnel and the flask washed twice with a small volume of EtOAc to ensure complete transfer of the solid into the funnel. The liquid was filtered through. The solid was triturated twice with Et2O and dried under vacuum to afford the desired product as a cream-colored solid (8.09 g, 17.9 mmol, 70.5 % yield). (M+H) = 452 m/e. H NMR (400 MHz, CHLOROFORM-d) delta ppm 1.44 (s, 9 H) 7.49 – 7.54 (m, 1 H) 7.54 (d, J=1.77 Hz, 1 H) 8.03 (d, J=5.31 Hz, 1 H) 8.30 (d, J=2.53 Hz, 1 H) 8.37 (d, J=5.31 Hz, 1 H) 9.98 (s, 1 H).

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

Reference£º
Patent; F. HOFFMANN-LA ROCHE AG; BROTHERTON-PLEISS, Christine; JAIME-FIGUEROA, Saul; LOPEZ-TAPIA, Francisco Javier; LOU, Yan; OWENS, Timothy D.; WO2013/24078; (2013); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

19064-74-5, 6-Bromophthalazine is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 17 N-(4-Methyl-3-phthalazin-6-yl-phenyl)-4-piperidin-1-ylmethyl-3-trifluoromethyl-benzamide Nitrogen is bubbled through a mixture of 0.295 g (0.648 mmol) N-(3-bromo-4-methyl-phenyl)-4-piperidin-1-ylmethyl-3-trifluoromethyl-benzamide, 0.191 g (1.94 mmol) potassium acetate and 0.198 g (0.778 mmol) bis-(pinacolato)-diboron in 3.12 mL DMF for about 10 minutes. After the addition of 0.032 g (0.0391 mmol) 1,1′-bis(diphenylphospino)ferrocene-palladium dichloride the mixture is heated to 80 C. for 6 h. The N-[4-methyl-3-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-4-piperidin-1-ylmethyl-3-trifluoromethyl-benzamide intermediate formed is not isolated. To the cooled dark suspension is added under nitrogen 6-bromophthalazine (0.1355 g, 0.648 mmol), caesium carbonate (0.316 g, 0.97 mmol) and 0.0225 mg (0.0195 mmol) tetrakis(triphenylphosphine)palladium. The dark mixture is heated to 80 C. for 15 h, cooled to rt and filtered. The solids are washed with DMF and the combined filtrates are evaporated under reduced pressure. The residue is partitioned between ethyl acetate and saturated sodium bicarbonate solution and the organic phase washed with brine, dried with sodium sulphate and evaporated. The crude product is purified by chromatography using a 40 g silica gel column on a Combi-Flash Companion (Isco Inc.) apparatus. A gradient of ethyl acetate/methanol (0?10% methanol) is used. Pure fractions are pooled and evaporated to give the title compound as tan crystals; m.p. 175-177 C.; Rf (ethyl acetate/methanol 9:1)=0.39; HPLC tR=2.50 min; MS-ES+: (M+H)+=505.

19064-74-5 6-Bromophthalazine 610436, aphthalazine compound, is more and more widely used in various.

Reference£º
Patent; Caravatti, Giorgio; Furet, Pascal; Imbach, Patricia; Martiny-Baron, Georg; Perez, Lawrence Blas; Sheng, Tao; US2006/35897; (2006); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.763111-47-3,4-(4-Fluoro-3-(piperazine-1-carbonyl)benzyl)phthalazin-1(2H)-one,as a common compound, the synthetic route is as follows.

4-[4-fluoro-3-(piperazin-1 -ylcarbonyl) benzyl] phthalazin-1 (2H)-one (IX) (40.0 g, 0.1 1 mol) and 1 H-benzotriazol-1 -yl(cyclopropyl)methanone (X) (26 g, 0.14 mol) were stirred in acetonitrile (320 mL) and the progress of reaction was monitored by HPLC. After completion of reaction, the resulted precipitate was filtered and washed with acetonitrile (40.0 mL) then dried to afford Olaparib (I) as a white to off- white solid. The PXRD pattern of Olaparib thus obtained matches with Form-A as illustrated in figure-3. (Yield: 90%, HPLC purity: 99.99%)

763111-47-3 4-(4-Fluoro-3-(piperazine-1-carbonyl)benzyl)phthalazin-1(2H)-one 11726399, aphthalazine compound, is more and more widely used in various.

Reference£º
Patent; ALEMBIC PHARMACEUTICALS LIMITED; SIRIPRAGADA, Mahender Rao; VELISOJU, Mahendar; ANEGONDI, Shreenivasa Prasad; JOSHI, Yogesh Vasant; PANWAR, Amit; PATEL, Malvika; (35 pag.)WO2017/191562; (2017); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.763111-47-3,4-(4-Fluoro-3-(piperazine-1-carbonyl)benzyl)phthalazin-1(2H)-one,as a common compound, the synthetic route is as follows.

4-(4-Fluoro-3-(piperazin-1-yl-carbonyl)-benzyl)pyridazine-1(2H)one (5) (0.78 g, 2.13 mmol) was added to a 25 ml three-necked flask.And adding dichloromethane (6.5 ml), 2-butynoic acid (215 mg, 2.56 mmol), HOBT (431 mg, 3.20 mmol), EDCI (614 mg, 3.20 mmol), and stirring to 1-10 C,An excess of DIPEA (550 mg, 4.26 mmol) was added dropwise and the mixture was allowed to warm to room temperature.After TLC showed that the reaction was completed, the reaction mixture was directly concentrated to dryness, and the residue was mixed with water and then stirred for 1 hour and then filtered.Obtained as an off-white solid.The yield was 31%.

As the paragraph descriping shows that 763111-47-3 is playing an increasingly important role.

Reference£º
Patent; Shanghai Bobang Pharmaceutical Technology Co., Ltd.; Gao Heyong; Liu Zhende; Zhang Wensheng; (28 pag.)CN108383798; (2018); A;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

89898-86-2, 5-Nitrophthalazine is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

B. A solution of 5-nitro-phthalazine (0.175 g, 1 mmol) and SnCl2 (0.57 g, 3 mmol) in concentrated HCl (10 mL) is stirred at room temperature for 2 h. Ice is added to the solution. A solution of 25% NaOH is added to pH 14 (litmus). The solution is cooled for 18 h. The solution is filtered. Aqueous filtrate is extracted twice with EtOAc. EtOAc layers are combined, washed with water, brine, dried over Na2SO4, filtered and concentrated to give phthalazin-5-ylamine (0.050 g).

As the paragraph descriping shows that 89898-86-2 is playing an increasingly important role.

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