Month: May 2021

59702-07-7, 1-Methylpiperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

59702-07-7, Intermediate 62 : 2-f3-f4-Methyl-3-oxopiperazin-l-vnpropynisoindoline-l,3- dione (0595) To a mixture of 3-(l,3-dioxoisoindolin-2-yl)propanal (515 mg, 2.53 mmol, commercially available from Fluorochem) and Na(OAc)3BH (815.9 mg, 3.85 mmol) in 2-MeTHF (20 mL) was added l-methylpiperazin-2-one (0.420 mL, 3.82 mmol, commercially available from Fluorochem). The mixture was stirred at rt for 4 h 45 min. To the reaction mixture was added aqueous 2M Na2C03 (10 mL) and this mixture stirred at rt for 10 min giving an aqueous phase at approximately pH 10. The layers were separated and the aqueous layer washed with EtOAc (2 x 10 mL). The organic layers were filtered through a cartridge fitted with a hydrophobic frit and the filtrate evaporated in vacuo to give a pale yellow crystalline solid. 2-(3-(4-methyl-3-oxopiperazin-l-yl)propyl)isoindoline-l,3-dione (660.5 mg, 2.192 mmol, 86 percent yield). (0596) LCMS (2 min high pH); Rt = 0.74 min, m/z = 302 for [MH]+

The synthetic route of 59702-07-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; ATKINSON, Stephen John; DEMONT, Emmanuel Hubert; HARRISON, Lee Andrew; LEVERNIER, Etienne; PRESTON, Alexander G; SEAL, Jonathan Thomas; WALL, Ian David; WATSON, Robert J; WOOLVEN, James Michael; (225 pag.)WO2017/174621; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.57260-70-5,tert-Butyl 4-benzylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

57260-70-5, The procedure described for the preparation of 2a was used with compound 10c (400 mg, 1.22 mmol), 13a (322 mg,1.83 mmol), K2CO3 (337 mg, 2.44 mmol), NaI (catalyst) and CH3CN(15 mL) to obtain 2c (296 mg, 52%) as light brown liquid. Rf = 0.56(n-hexane: EtOAc: MeOH = 2.5:1.5:1). 1H NMR (500 MHz, CDCl3): d7.38-7.23 (m, 15H), 5.86 (s, 1H), 4.61 (t, J = 7 Hz, 2H), 3.54 (s, 2H),2.48-2.00 (m, 10H), 2.07-2.02 (m, 2H), 1.52-1.49 (m, 2H); 13CNMR (125 MHz, CDCl3): d 167.8, 140.9, 138.2, 129.2, 128.7, 128.6,128.2, 127.1, 127.0, 63.1, 57.6, 53.2, 53.1, 53.0, 48.7, 27.4, 23.6.

57260-70-5 tert-Butyl 4-benzylpiperazine-1-carboxylate 584330, apiperazines compound, is more and more widely used in various fields.

Reference£º
Article; Paudel, Suresh; Acharya, Srijan; Yoon, Goo; Kim, Kyeong-Man; Cheon, Seung Hoon; Bioorganic and Medicinal Chemistry; vol. 25; 7; (2017); p. 2266 – 2276;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

115761-79-0, 1-(2,4-Difluorophenyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A solution of Intermediate?A? (200 mg, 0.55 mmol), l-(2,4-difluorophenyl)- piperazine (328 mg, 1.65 mmol), and Et3N (170 mg) in CH2CI2 (5 g) was stirred for 16 h at rt, then extracted with 2×30 mL of CH2CI2. The combined organic layers were concentrated under vacuum and purified with silica gel column chromatography using EtOAc / hexane (1:1) to afford 240 mg (97%) of the title compound as an off-white solid. LC-MS: (ES, m/z): 449.

115761-79-0, As the paragraph descriping shows that 115761-79-0 is playing an increasingly important role.

Reference£º
Patent; CENTAURUS THERAPEUTICS; ROMERO, Donna, L.; BLITZER, Jeremy; (242 pag.)WO2019/140188; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

59878-57-8, 1-(Cyclopropylcarbonyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,59878-57-8

INTERMEDIATE 48(S)-tert~BvLtyl 1 – { 8-chloro-2- F4-C cvclopropanecarbonvDpiperazin- 1 -yl] quinolin-3- vDethylcarbamateIntermediate 11 (150 mg, 0.44 mmol), cyclopropyl(piperazin-l-yl)methanone (0.16 mL, 1.1 mmol), NMP (2 mL) and DIPEA (0.38 mL, 2.2 mmol) were combined in a sealed tube and heated to 14O0C for 36 h. After cooling, Et2O was added to the reaction mixture. The organic layer was washed with water and brine. The organic layer was dried (MgSO4), filtered and the solvent was removed in vacuo. Purification by column chromatography on silica, eluting with 0-5% MeOH in EtOAc, gave the title compound (175 mg, 86%) as a yellow gum. deltaH (CDCl3) 8.00 (IH, s), 7.71 (IH, dd, J7.5, 1.3 Hz), 7.62 (IH, dd, J8.1, 1.3 Hz), 7.34-7.28 (IH, m), 5.15 (IH, br s), 4.95 (IH, br s), 3.86 (4H, br s), 3.60 (2H, br s), 3.34 (2H, br s), 1.85-1.77 (IH, m), 1.46 (3H, s), 1.44 (9H, s), 1.05- 1.00 (2H, m), 0.80 (2H, dd, J 7.8, 3.5 Hz). LCMS (ES+) 459 (M+H)+.

59878-57-8 1-(Cyclopropylcarbonyl)piperazine 2064235, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; UCB PHARMA S.A.; ALLEN, Daniel, Rees; BUeRLI, Roland; HAUGHAN, Alan, Findlay; MACDONALD, Jonathan, David; MATTEUCCI, Mizio; NASH, David, John; OWENS, Andrew, Pate; RAPHY, Gilles; SAVILLE-STONES, Elizabeth, Anne; SHARPE, Andrew; WO2010/100405; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.115761-79-0,1-(2,4-Difluorophenyl)piperazine,as a common compound, the synthetic route is as follows.

General procedure: A mixture of 3 (100 mg, 0.28 mmol), arylpiperazines or piperidines,K2CO3, (1.2 equiv), potassium carbonate (6.0 equiv) and CH3CN(25 mL) were placed in 50-mL round-bottomed flask equipped withmagnetic stirrer for 14 h at 85 C (monitored by TLC). After completionof reaction, the reaction mixture was filtered, and the filtrate wasconcentrated in vacuo. Then the residue was purified by chromatographyon silica-gel column (petroleum ether: ethyl acetate=5:1, v/v)to obtain the corresponding products (4-26), and all compounds wererecrystallized from dichloromethane and n-hexane., 115761-79-0

The synthetic route of 115761-79-0 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Chen, Hong; Liang, Xue; Sun, Tao; Qiao, Xiaoguang; Zhan, Zhou; Li, Ziyong; He, Chaojun; Ya, Huiyuan; Yuan, Mu; Steroids; vol. 134; (2018); p. 101 – 109;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.262368-30-9,N-(4-Aminophenyl)-N-methyl-2-(4-methylpiperazin-1-yl)acetamide,as a common compound, the synthetic route is as follows.

A mixture of the compound of formula V (lOg) and N-(4-aminophenyl)-N-methyl-2-(4- methylpiperazin-l-yl)acetamide (formula IV) (7.89g) in DMF (50ml) was stirred at about 65-70C for 4h. The reaction mass was cooled to about 25-30C and stirred for lh. Reaction mass was filtered and solid was washed with methanol. The solid wet cake was added in methanol and stirred at about 25-30C. Reaction mass was cooled to about 0-5C and piperidine (6.2ml) was added under stirring. The reaction mass was heated to about 25-30C and stirred for 5h. The reaction mass was cooled to about 0-5C and stirred for lh. The reaction mass was filtered and solid was washed with cold methanol to obtain crude nintedanib. Yield: 12gm; HPLC purity: 99.96%; Imp B: 0.02%.

262368-30-9, The synthetic route of 262368-30-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; GLENMARK PHARMACEUTICALS LIMITED; NAIK, Samir; SRIVASTAVA, Sachin; PATIL, Pramod; PATIL, Premchand Bansilal; BHIRUD, Shekhar Bhaskar; (34 pag.)WO2019/48974; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.75336-86-6,(R)-2-Methylpiperazine,as a common compound, the synthetic route is as follows.

75336-86-6, To the 1200 L reactor was dissolved (R)-2-methylpiperazine from Example 5 (25 kg) in CH3CN (319 kg) at [15¡ãC] to [25¡ãC] until dissolution was complete (10 min. ) After cooling to [5¡ãC] to [10¡ãC] Et3N (63 kg) was added. To the 1200 L receiver trityl chloride (69.5 kg) was dissolved in CH2C12 (106 kg) at [15¡ãC] to [25¡ãC.] The solution in the receiver was transferred to the reactor over 0.5 h with a CH2C12 rinse (27 kg), and the solution was heated to [20¡ãC] to [30¡ãC.] The reaction was monitored by GLC and was complete in 1 h. The resulting slurry was cooled to [8¡ãC] to [12¡ãC,] filtered onto a 48″Nutsche filter, and rinsed with CH3CN (40 kg at [8¡ãC] to [12¡ãC).] The filter cake was dried using [50¡ãC] to [55¡ãC] nitrogen to afford 25.26 kg of the by-product [ET3NHCL] (74percent yield; easy to filter off the by-product). The filtrate was transferred to the 1200 L reactor and cooled further [TO-8¡ãC] [TO-10¡ãC] for 1 h. The resulting slurry was filtered onto a 24″Nutsche filter and rinsed [WITH-8¡ãC] to-10¡ãC CH3CN (24 kg) sending the filtrate and rinse to the 1200 L receiver. The filter cake was dried with [50¡ãC] to [55¡ãC] nitrogen to afford another 2.98 kg [ET3NHCL] (9percent yield). The filtrate was transferred to the 1200 L reactor with a CH3CN (10 kg) rinse, and distilled under vacuum to an oil of the title compound of 97.99percent GC purity. The yield was quantitative. M. Pt. [134-136¡ãC.] [APOS;H] NMR (400 MHz, CDC13) : [6] 7.55-7. 40 (6H, br s), 7.25 (6H, t, J = 7. 9 Hz), 7.14 (3H, t, [J =] 7.1 Hz), 3.21-3. 13 (2H, [M),] 3. [10-2. 90 (1H,] br s), 2.94 (2H, t, J = 13.0 Hz), 1.60 [(1H,] br s), 1.48 (1H, br s), 1.15 (1H, br s), 0.94 (3H, d, J = 6.1 Hz), 0.00 (TMS, reference). [13C] NMR (100 MHz, CDC13) : [6] 129.41 (d), 127.46 (d), 125.96 (d), 125.83 (s), 56.12 (t), 51.23 (d), 48.73 (t), 46.45 (t), 20.05 (q), 0.00 (TMS, reference). IR (diffuse reflectance) 2964,2835, 2483 (w), 2350 (w), 2339 (w), 1956 (w), 1490,1025, 909,742 (s), 717,710 (s), 703 (s), 697 (s), 629, [CM-1.] HRMS [(EI)] calcd for [C24H26N2] 342.2096, found [342. 2101.] [a] [25D=-12¡ã (C 1. 00, CH2CL2).] Anal. Calcd for [C24H26N2] : C, 84.17 ; H, 7.65 ; N, 8.18. Found: C, 84.12 ; H, 7.64 ; N, 7.94.

75336-86-6 (R)-2-Methylpiperazine 7330434, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; BIOVITRUM AB; WO2004/829; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.31321-68-3,(R)-Piperazine-2-carboxylic acid,as a common compound, the synthetic route is as follows.

To a solution of (R)-piperazine-2-carboxylic acid (70 g, 344.71 mmol, 1.0 equiv, 2HCl) in dioxane (1120 mL) and H2O (700 mL) was added 50% aq. NaOH until the solution was pH=11. Benzyl chloroformate (156.82 mL, 1.10 mol, 3.2 equiv) was added and the reaction mixture was stirred at room temperature for 12 h. To the solution was then added H2O (1200 mL) and the aqueous layer was washed with MTBE (3 x 800 mL). The aqueous layer was adjusted to pH=2 with concentrated HCl (12N) and extracted with EtOAc (2 x 1000 mL). The combined organic extracts were dried, filtered and the filtrate was concentrated under reduced pressure to afford the desired product (137 g, 99.8% yield) as a yellow solid. LCMS (ESI) m/z: [M + H] calcd for C21H22N2O6: 399.16; found 399.2., 31321-68-3

31321-68-3 (R)-Piperazine-2-carboxylic acid 6558437, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; REVOLUTION MEDICINES, INC.; PITZEN, Jennifer; GLIEDT, Micah James Evans; BURNETT, G. Leslie; AGGEN, James Bradley; KISS, Gert; CREGG, James Joseph; SEMKO, Christopher Michael; WON, Walter; WANG, Gang; LEE, Julie Chu-Li; THOTTUMKARA, Arun P.; GILL, Adrian Liam; MELLEM, Kevin T.; (484 pag.)WO2019/212990; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.57260-71-6,tert-Butyl piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

Step 1 : tert-Butyl 4-benzylpiperazine-l-carboxylate (0754) [00268] To a solution of compound A3-1 (20.0 g, 107 mmol, 1.0 eq) and (0755) bromomethylbenzene (22.0 g, 129 mmol, 1.2 eq) in CH3CN (300 mL) was added K2CO3 (14.8 g, 107 mmol, 1.0 eq). The reaction mixture was stirred at 70 C for 16 hours. The reaction mixture was concentrated under reduced pressure. The mixture was diluted with water (50 mL) and the resultant mixture was extracted with EA (80 mL * 2). The combined organic layers were dried over NaiSO/t, filtered and concentrated to dryness under reduced pressure. The residue was purified by column chromatography over silica gel (petroleum ether: ethyl acetate = 1 :0 to 5: 1) to afford the title compound (16.8 g, 57% yield) as a white solid. ‘HNMR (400MHZ, CDCl3-i/) delta 7.34 – 7.23 (m, 5H), 3.50 (s, 2H), 3.46 – 3.38 (m, 4H), 2.43 – 2.33 (m, 4H), 1.45 (s, 9H), 57260-71-6

The synthetic route of 57260-71-6 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; VIVACE THERAPEUTICS, INC.; LIN, Tracy Tzu-Ling Tang; KONRADI, Andrei W.; VACCA, Joseph; SHEN, Wang; COBURN, Craig; (231 pag.)WO2017/58716; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.103-76-4,N-(2-Hydroxyethyl)piperazine,as a common compound, the synthetic route is as follows.,103-76-4

2-(4-Methylpiperazin-l-yl)ethyl 4-nitrophenyl carbonate To a stirred solution of l-(2-hydroxyethyl)piperazine (26.0 g, 0.2 mol) in DMF (200 mL) was added formic acid (752 mL, 0.2 mol) and formaldehyde (16.2 g, 0.2 mol, 37% solution in water) The reaction mixture was cautiously heated at 100 0C for 2 hours and then stirred overnight at room temperature. The solvent was removed in vacuo. This procedure was repeated 3 further times to give -100 g of product. The crude products were combined and distilled under vacuum to give, at ~74 0C, 2-(4-methylpiperazin-l-yl)ethanol (51 g, 44%) as a colourless liquid. Analytical LCMS: (System B, Rtau = 0.70 min), ES+: 145.1 (100%) [MH]+.

The synthetic route of 103-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; BIOVITRUM AB (publ); WO2009/71677; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics