Month: August 2020

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.

In a 10ml seal tube, 6-bromo-2H-pyridazin-l-one (108 mg, 480 muetaiotaomicron, Eq: 1.00), NH4OH (931 mg, 1.03 ml, 7.97 mmol, Eq: 16.6) and copper powder (30.5 mg, 480 muiotaetaomicron, Eq: 1.00) were combined with isopropyl alcohol (1 ml) to give a light brown suspension. The tube was sealed and the reaction was heated to 100 C overnight. The crude reaction mixture was concentrated in vacuo. The reaction mixture was diluted with sat NH4C1 and dichloromethane. The 2 phase mixture was filtered, the filtrate was separated and the aqueous extracted with dichloromethane (3X30 ml). SiC”2 was added to the aqueous phase and concentrated. The solid was suspended in hot dichloromethane/methanol 9: 1 and sonicated. Filtered and washed the filter cake with warm dichloromethane/methanol 9: 1. The filtrate was combined with the dichloromethane extracts and stripped to a light yellow powder. The powder was dried under vacuum at 25C for 1 hour to afford 62 mg (80%) of the desired product. MS +m/z: 162.1. (M+l)

The synthetic route of 75884-70-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; CHEN, Zhi; CHIN, Elbert; ERICKSON, Shawn David; GABRIEL, Stephen Deems; MERTZ, Eric; WEIKERT, Robert James; WO2014/135483; (2014); 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.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, acryloyl chloride (230 mg, 2.56 mmol) was added dropwise, and the mixture was warmed to room temperature and stirred for 1 h.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%.

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

152265-57-1, 7-Bromophthalazin-1(2H)-one is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A mixture of 7-bromo-l,2-dihydrophthalazin-l-one (4.1 g, 18.22 mmol) and bis(pinacolato)diboron (12.95 g, 51.01 mmol) was dissolved in 1,4-dioxane (150 mL) under nitrogen. Potassium acetate (5.36 g, 54.66 mmol) was added, and the reaction mixture was degassed with N2 for 5 minutes. Pd(dppf)Cl2 (0.74 g, 0.91 mmol) was added and the mixture was heated at 110C for 1.5 h, then cooled and diluted with DCM. The solids were removed by filtration through celite. The residue was washed with DCM and the combined organic phases were concentrated in vacuo. The resulting solid was triturated in heptane (30 mL) and diethyl ether (15 mL). The solid was further triturated with heptane (30 mL) and diethyl ether (15 mL), then the precipitate was collected by filtration, to give the title compound (5.1 g, 81%). deltaEta (250 MHz, DMSO-d6) 12.68 (s, 1H), 8.50 (s, 1H), 8.37 (s, 1H), 8.10 (dd, J7.8, 1.1 Hz, 1H), 7.88 (d, J7.8 Hz, 1H), 1.30 (s, 12H). Method B: HPLC-MS MH+ mlz 273, RT 1.78 minutes (97%)

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

Reference£º
Patent; UCB BIOPHARMA SPRL; BRACE, Gareth Neil; CHOVATIA, Prafulkumar Tulshibhai; FOULKES, Gregory; JOHNSON, James Andrew; JONES, Severine Danielle; KROEPLIEN, Boris; LECOMTE, Fabien Claude; LOKE, Pui Leng; LOWE, Martin Alexander; MANDAL, Ajay; NORMAN, Timothy John; PALMER, Christopher Francis; PEREZ-FUERTES, Yolanda; PORTER, John Robert; SMYTH, Donald; TRANI, Giancarlo; UDDIN, Muhammed; ZHU, Zhaoning; (207 pag.)WO2016/198400; (2016); 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.75884-70-7,6-Bromophthalazin-1(2H)-one,as a common compound, the synthetic route is as follows.

A solution of 6-bromophthalazine-1(2H)-one (0.25 g, 1.11 mmol), potassium vinyl trifluoroborate (0.446 g, 3.33 mmol) and K2CO3 (0.46 g, 3.33 mmol) in DMSO (2 mL) was degassed with argon for 20 min at RT. PdCl2(dppf) (0.04 g, 0.055 mmol) was added at RT, and the reaction mixture was heated to 80 C for 2 h. The reaction mixture was cooled to RT and filtered through celite bed under vacuum and washed with ethyl acetate. The reaction mixture was extracted with ethyl acetate and the combined ethyl acetate layer dried over Na2S04 and concentrated under reduced pressure to afford the crude product. The crude compound was purified by column chromatography (Si02, 100-200 mesh; 50% ethyl acetate/ petroleum ether) to afford the title compound as a brown solid (0.12 g, 63%): ]H NMR (400 MHz, DMSO-d6) delta 13.61 (br, 1H), 8.33 (m, 1H), 8.19 (m, 1H), 8.01 (m, 2H), 6.97 (m, 1H), 6.15 (m, 1H), 5.56 (d, / = 10.8 Hz, 1H); ESIMS m/z 172.93 ([M+H] +); IR (thin film) 1748, 1655, 3241 cm”1

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

Reference£º
Patent; DOW AGROSCIENCES LLC; LO, William, C.; HUNTER, James, E.; WATSON, Gerald, B.; PATNY, Akshay; IYER, Pravin, S.; BORUWA, Joshodeep; WO2014/100206; (2014); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

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

6-Bromo-2,3-dihydrophthalazine-1 ,4-dione (25. g, 0.10 mol) was added to a mixture of phosphorus oxychloride (100. mL, 1 .06 mol) and thionyl chloride (100. mL, 1 .37 mol) under nitrogen, cooled to 0 C. Once the initial exotherm had subsided the reaction mixture was allowed to warm to ambient temperature and then heated at 100 C for 4 h. The mixture was then cooled to ambient temperature and then concentrated in vacuo. The residue was dissolved in iPrOAc (350 mL) and washed with saturated sodium bicarbonate solution (added until effervescence stopped), a precipitate formed, the two layers were filtered to isolate the first crop of the intermediate. The organic layer was collected and distilled to dryness to give the second crop of the intermediate. The solids were combined and partitioned between 1 ,4-dioxane (200 mL) and 2 N NaOH (100 mL). The resulting mixture was heated at 40 C overnight and then cooled to ambient temperature and left to stand. The solid precipitate was filtered (first crop of product) and the resulting solution partitioned between EtOAc (250 mL) and water (200 mL). Further precipitate formed which was filtered and combined with the first crop of the product, the organic phase was separated and evaporated to dryness to give the second crop of the product. Product isolated is a mixture of two regioisomers, 7-bromo-4-chloro-2H-phthalazin-1 -one and 6- bromo-4-chloro-2H-phthalazin-1 -one, total yield isolated (17.6 g, 68.0 mmol, 66%).1 H NMR (300MHz, DMSO-d6) delta = 13.02 (s, 1 H), 12.98 (s, 1 H), 8.36 (d, J = 2.1 Hz, 1 H), 8.22 (dd, J = 2.1 , 8.6 Hz, 1 H), 8.17 – 8.1 1 (m, 3H), 7.93 (d, J = 8.7 Hz, 1 H). 1 :1 mixture of the two regioisomers.

As the paragraph descriping shows that 76240-49-8 is playing an increasingly important role.

Reference£º
Patent; CANCER RESEARCH TECHNOLOGY LIMITED; MCGONAGLE, Alison E.; JORDAN, Allan; WASZKOWYCZ, Bohdan; HUTTON, Colin; WADDELL, Ian; HITCHIN, James R.; SMITH, Kate Mary; HAMILTON, Niall M.; (497 pag.)WO2016/92326; (2016); 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.19064-74-5,6-Bromophthalazine,as a common compound, the synthetic route is as follows.

EXAMPLE 40; N-(2-chloro-5-(6-phthalazinyl)-3-pyridinyl)-4-fluorobenzenesulfonamide; A suspension of N-(2-chloro-5-(4,4,5,5-tetramethyl-l,3,2-dioxaborolan-2- yl)pyridin-3-yl)-4-fluorobenzenesulfonamide (102 mg, 247 mumol), 6-bromophthalazine (43 mg, 206 mumol), dichloro[l,rbis(diphenylphoshino)ferrocene]palladium(II)dichloromethane adduct (11 mg, 15 mumol), and Na2CO3 (65 mg, 617 mumol) in 1,4-dioxane (2 mL) and water (1 mL) was sparged with nitrogen for 5 minutes, then heated to 100 0C for 2 hours. The reaction was then partitioned between 9: 1 CHC13/IPA (30 mL) and 5% NaHCO3 (10 mL). The separated organic was dried over Na2SO4, concentrated onto dry silica, and then purified on silica eluting with 2- >5% of MeOH/DCM. Product was isolated as light yellow solid. MS (ESI pos. ion) m/z calc’d for Ci9H12ClFN4O2S: 414.0; found 415.0. 1H NMR (400 MHz, DMSO-d6) delta 7.44 (t, J=8.8 Hz, 2 H) 7.80 – 7.87 (m, 2 H) 8.24 (d, J=2.1 Hz, 1 H) 8.32 (d, J=8.4 Hz, 1 H) 8.38 (dd, J=8.7, 2.0 Hz, 1 H) 8.54 (s, 1 H) 8.79 (d, J= 2.1 Hz, 1 H) 9.76 (s, 2 H) 10.60 (s, 1 H).

As the paragraph descriping shows that 19064-74-5 is playing an increasingly important role.

Reference£º
Patent; AMGEN INC.; WO2009/155121; (2009); A2;,
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

Step 3. 6-Vinylphthalazine-1(2H)-one (BI27) A solution of 6-bromophthalazine-1(2H)-one (0.25 g, 1.11 mmol), potassium vinyl trifluoroborate (0.446 g, 3.33 mmol) and K2CO3 (0.46 g, 3.33 mmol) in DMSO (2 mL) was degassed with argon for 20 min at ambient temperature. PdCl2(dppf) (0.04 g, 0.055 mmol) was added at ambient temperature, and the reaction mixture was heated to 80 C. for 2 h. The reaction mixture was cooled to ambient temperature and filtered through celite bed under vacuum and washed with ethyl acetate. The reaction mixture was extracted with ethyl acetate and the combined ethyl acetate layer dried over Na2SO4 and concentrated under reduced pressure to afford the crude product. The crude compound was purified by column chromatography (SiO2, 100-200 mesh; 50% ethyl acetate/petroleum ether) to afford the title compound as a brown solid (0.12 g, 63%): 1H NMR (400 MHz, DMSO-d6) delta 13.61 (br, 1H), 8.33 (m, 1H), 8.19 (m, 1H), 8.01 (m, 2H), 6.97 (m, 1H), 6.15 (m, 1H), 5.56 (d, J=10.8 Hz, 1H); ESIMS m/z 172.93 ([M+H]+); IR (thin film) 1748, 1655, 3241 cm-1.

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

Reference£º
Patent; Dow AgroSciences LLC; Lo, William C.; Hunter, James E.; Watson, Gerald B.; Patny, Akshay; Iyer, Pravin S.; Boruwa, Joshodeep; US9211280; (2015); B2;,
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

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.Propionyl chloride (236 mg, 2.56 mmol) was added dropwise, and the mixture was warmed to room temperature and stirred for 1 h.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 50%.

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;,
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.

The dried radiola beled 131l-N HS-benzoate precursor was dissolved in 200 mu of acetonitrile and an excess of H BTU (1 mg, 2.6 nmol) and 4-(4-fluoro-3-(piperazine-l-carbonyl)benzyl)phthalazin- l(2H)-one (1 mg, 2.7 nmol) was added and allowed to react for 3 h at 32 C. The final product was purified by H PLC, using water and acetonitrile as solvents with a gradient elution from 5% to 100% of solvent B over 15 min and then 100% of B from 15 to 25 min. The retention time of C-2d was 13.1 min and its identity was esta blished by co-elution with the reference cold compound. The radiochemical yield was 72 ¡À 8 % (n=12) and the radiochemical purity > 95%. The collected fraction containing C-2d was concentrated to dryness under reduced pressure

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

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;,
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.

(c) 4-[3-(4-Cyclopropanecarbonyl-piperazine-1-carbonyl)-4-fluoro-benzyl]-2H-phthalazin-1-one (A)To a stirred suspension of compound B (1290 g) in CH2CI2 (15480 ml) under nitrogen was added a pre-mixed solution of triethylamine (470 ml) and cyclopropane carbonyl chloride (306 ml) in CH2CI2 (1290 ml) dropwise with the temperature kept below 2O0C. The solution was then stirred at 10-15C for 15 minutes and sampled for completion. The reaction mixture was found to contain only 1.18% of starting material B and so the reaction was deemed complete and the batch was then worked-up.The reaction mixture was washed with water (7595 ml), 5% citric acid solution (7595 ml), 5% sodium carbonate solution (7595 ml) and water (7595 ml). The organic layer was then dried over magnesium sulfate (50Og).The CH2CI2 containing product layer was then isolated, filtered through Celite and charged to a 25I vessel. CH2CI2 (8445 ml) was then distilled out at atmospheric pressure and ethanol (10000 ml) added. Distillation was then continued with every 4000 ml of distillate that was removed being replaced with ethanol (4000 ml) until the head temperature reached 73.70C. The reaction volume was then reduced (to 7730 ml) by which time the head temperature had reached 78.90C and the solution was allowed to cool to 8C overnight. The solid was then filtered off, washed with ethanol (1290 ml) and dried at 700C overnight.Yield = 1377.3 g (90%). HPLC purity (99.34% [area %]). Contained 4.93% ethanol and 0.45% CH2CI2 by GC.

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

Reference£º
Patent; KUDOS PHARMACEUTICALS LIMITED; WO2008/47082; (2008); A2;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem