Month: September 2021

109-07-9, 2-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 1 In a 100 ml four-neck flask, 5.00 g (= 0.0499 mole) of racemic 2-methylpiperazine was placed, and 44 g of 1-butanol (water content 0.05 wt%) was added for dissolution. The solution was cooled to 0C, and 8.47 g of benzyl chlorocarbonate (= 0.0489 mole, purity by HPLC determination analysis 98.5 wt%, 0.98 molar time) was added dropwise in a liquid temperature range from 0 to 8C. Then, stirring was carried out at 0 to 5C for 2 hours, and the reaction solution was partially sampled and determined by the internal standard method (internal standard: anisole). As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 83.9% (based on the amount of 2-methylpiperazine). The reaction solution was further stirred at room temperature for 12 hours and analyzed. As a result, the reaction yield was 85.1%. Example 3 A reaction was performed as described for Example 1, except that the amount of benzyl chlorocarbonate used was changed from 8.47 g to 10.1 g (= 0.0597 mole, 1.17 molar times). As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 93.8% (based on the amount of 2-methylpiperazine) after lapse of 2 hours at 0 to 5C. Stirring was carried out at room temperature for further 12 hours, being followed by analysis. As a result, the reaction yield was 95.1%., 109-07-9

As the paragraph descriping shows that 109-07-9 is playing an increasingly important role.

Reference：
Patent; Toray Fine Chemicals Co., Ltd.; EP1548010; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

50606-32-1,50606-32-1, Butyl piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

50.3. 4-[(R)-2-tert-Butoxycarbonylamino-3-(diethoxy-phosphoryl)-propionyl]-piperazine-l- carboxylic acid butyl ester: To a solution of intermediate 50.2 (7.37 g) in DCM (95 mL), THF (24 mL) and DIPEA (16.3 mL) were added HOBT (3.83 g) and EDC-HCl (4.78 g), and the reaction mixture was stirred at RT for 10 min. Subsequently, piperazine- 1 -carboxylic acid butyl ester (5.31 g) was added and the mixture stirred at RT for 2.5 h. The reaction mixture was diluted with DCM, the org. phase washed with sat. aq. NaHCO3 and the aq. phase re-extracted with DCM. The combined org. phases were washed with brine, dried over Na2SO^ and concentrated to dryness. Purification by CC (EtOAc/MeOH 1:0 to 9: 1) gave 7.66 g of the desired product. LC-MS: tR = 0.94 min; [M+H]+: 494.00

50606-32-1 Butyl piperazine-1-carboxylate 21963126, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; ACTELION PHARMACEUTICALS LTD; CAROFF, Eva; HILPERT, Kurt; HUBLER, Francis; MEYER, Emmanuel; RENNEBERG, Dorte; WO2010/116328; (2010); A2;,
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.109384-27-2,1-Methylpiperazin-2-one hydrochloride,as a common compound, the synthetic route is as follows.

[0348] Methyl-2-piperazinone hydrochloride (1:1) (300 mg, 1.99 mmol) was combined with dichloromethane (20 mL) to give a light yellow suspension. N,N-Diisopropylethylamine (309 mg, 417 mul, 2.39 mmol) was added at 0 C. Subsequently 3-(4-cyanophenyl)-2-oxaziridinecarboxylic acid 1,1-dimethylethyl ester (441 mg, 1.79 mmol) in dichloromethane (10 mL) was added during 35 min at 0 C. and the reaction mixture was stirred for 1 h at 0 C. Afterwards the reaction mixture was concentrated in vacuo and the residue was purified by flash chromatography (silica gel, 20 g, 0% to 100% ethyl acetate in n-heptane) to deliver an oil contaminated with 4-cyano-benzaldehyde. This material was purified by a second chromatography (aminophase 5 g, ethyl acetate/n-heptane 1/1) to give the title compound (67 mg, 15%) as white solid; GC-MS (EI) 229.0 (M)+

109384-27-2, 109384-27-2 1-Methylpiperazin-2-one hydrochloride 17060766, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Grether, Uwe; Hebeisen, Paul; Mohr, Peter; Ricklin, Fabienne; Roever, Stephan; US2013/65876; (2013); 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.30459-17-7,1-(4-Trifluoromethylphenyl)piperazine,as a common compound, the synthetic route is as follows.

A solution of Intermediate?A? (200 mg, 0.55 mmol), l-[4-(trifluoromethyl)- phenyl | piperazine (381 mg, 1.65 mmol), and Et3N (170 mg, 1.68 mmol) in CH2CI2 (5 mL) was stirred for 16 h at rt, then extracted with 2×20 mL of CH2CI2. The combined organic layers were concentrated under vacuum and purified with silica gel column chromatography using EtOAc / hexane (1:2) to afford 260 mg (98%) of the title compound as an off-white solid. LC-MS: (ES, m/z): 481

30459-17-7, As the paragraph descriping shows that 30459-17-7 is playing an increasingly important role.

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

55121-99-8, (4-Aminophenyl)(4-methylpiperazin-1-yl)methanone is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,55121-99-8

Example 164 N-[4-(4-Methylpiperazin-1-ylcarbonyl)phenyl]-(2-chloro-5-nitrophenyl)carboxamide The title compound (0.54 g, yield 89%) was obtained according to the procedure described in Example 2 using 4-(4-methylpiperazin-1-ylcarbonyl)aniline (0.33 g, 1.50 mmol), DMA (5 ml) and 2-chloro-5-nitrobenzoyl chloride (0.40 g, 1.80 mmol). 1H-NMR (400 MHz, DMSO-d6, TMS): delta(ppm) 2.32 (4H, m), 3.34-3.59 (4H, m), 7.42 (2H, d, J=8.6 Hz), 7.77 (2H, d, J=8.6 Hz), 7.91 (1H, d, J=8.8 Hz), 8.35 (1H, dd, J=2.7, 8.8 Hz), 8.49 (1H, d, J=2.7 Hz), 10.89 (1H, s); MS(FAB) m/z: 403 (M+H)+.

The synthetic route of 55121-99-8 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; SANKYO COMPANY, LIMITED; US2003/134859; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

314741-39-4, (S)-1-tert-Butyl 3-methyl piperazine-1,3-dicarboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,314741-39-4

1-tert-Butyl 3-methyl (3S)-piperazine-1,3-dicarboxylate (10 g, 40.9 mmol), (4-fluorophenyl)boronic acid (11.5 g, 82.1 mmol), copper(II) acetate (7.44 g, 40.9 mmol) and pyridine (6.67 ml, 82.6 mmol) were suspended in anhydrous 1,2-dichloroethane (300 ml) and the mixture was stirred at ambient temperature for 72 hours. A continuous airflow was bubbled through the reaction and the mixture stirred for 44 hours at ambient temperature. The airflow was removed and the reaction stirred at 45 C. for 20 hours, then cooled to ambient temperature. The mixture was filtered through celite, washed with DCM. The filtrate was concentrated in vacuo and the green oil obtained was purified via flash column chromatography eluting with gradient from 0-100% EtOAc in heptane followed by 0-100% MeOH in EtOAc. The product containing fractions were combined and concentrated in vacuo to afford the title compound as a yellow oil (4.29 g, 29%). 1H NMR (500 MHz, Chloroform-d) delta 6.98-6.92 (m, 2H), 6.85-6.80 (m, 2H), 4.47 (d, J=12.7 Hz, 1H), 4.27 (s, 1H), 4.21-3.92 (m, 1H), 3.64 (s, 3H), 3.60-3.47 (m, 1H), 3.37 (d, J=10.6 Hz, 1H), 3.27-2.99 (m, 2H), 1.46 (s, 9H). LCMS Method 3 Tr=1.88 min, (ES+) (M+H+)339.1.

As the paragraph descriping shows that 314741-39-4 is playing an increasingly important role.

Reference：
Patent; Navitor Pharmaceuticals, Inc.; O’Neill, David John; Saiah, Eddine; Kang, Seong Woo Anthony; Brearley, Andrew; Bentley, Jonathan; (519 pag.)US2018/127370; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

438049-35-5, N-Boc-3-Ethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step 3-1, Preparation of tert-butyl (3R)-3-ethyl-4-[3-fluoro-2-(methoxycarbonyl)-4-nitrophenyl]piperazine-1-carboxylate To a solution of tert-butyl-(3R)-3-ethylpiperazine-1-carboxylate (555 mg, 2.59 mmol) and methyl 2,6-difluoro-3-nitrobenzoate (843 mg, 3.89 mmol) in DMSO (2 mL) was added DIEA (0.90 mL, 5.2 mmol). The mixture was heated at 130 C. for 1 h. The mixture was purified by C18 reversed phase column chromatography to give the title compound (813 mg, 76% yield) as a brownish yellow gum. LCMS (M+H)+: 412.3., 438049-35-5

The synthetic route of 438049-35-5 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Crinetics Pharmaceuticals, Inc.; HAN, Sangdon; ZHU, Yunfei; KIM, Sun Hee; ZHAO, Jian; WANG, Shimiao; (146 pag.)US2019/367481; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5464-12-0,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5464-12-0,1-(2-Hydroxyethyl)-4-methylpiperazine,as a common compound, the synthetic route is as follows.

Sodium hydride (60percent, 0.87 g, 21.80 mmol) was added to diglyme (10 mL). A solution of 2-(4-methyl-piperazin-1-yl)-ethanol (3.14 g, 21.80 mmol) in diglyme (10 mL) was added slowly. The reaction mixture was heated at 40 00 for 1 hour, 4-chloro-pyridin- 2-ylamine (1.40 g, 10.9 mmol) was added and the reaction mixture was heated at 8000 for 1 hour, then at 15700 for 16 hours. The reaction mixture was cooled, diluted with water (20 mL), and THF (20 mL) was added, then NaCI. The organic phase was separated, and the aqueous phase was extracted with THF. The combined organic phase was dried, and the solvent was evaporated. Diethyl ether was added to the residue. The resulting solid was filtered, washed with ether, and dried to afford a white solid (1.86 g, 72percent), (M+H)=237.

The synthetic route of 5464-12-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ASTEX THERAPEUTICS LIMITED; SAXTY, Gordon; MURRAY, Christopher William; BERDINI, Valerio; PAGE, Lee William; ROOMANS, Susan; TAMANINI, Emiliano; BUCK, Ildiko Maria; DAY, James Edward Harvey; CARR, Maria Grazia; LEE, Lydia Yuen Wah; WO2015/4481; (2015); 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.57184-25-5,1-(Cyclopropylmethyl)piperazine,as a common compound, the synthetic route is as follows.

4-Cyclopropylmethyl-piperazine-1-carboxylic Acid 4-[2-(4-chloro-phenyl)-ethylcarbamoyl]-phenyl Ester The title compound was prepared from 4-[2-(4-chloro-phenyl)-ethylcarbamoyl]-phenyl chloroformate and 1-cyclopropylmethyl-piperazine, yield 18%. White crystals, m.p. 225-226 C.; IR (KBr): nu 1710 (ester C=O), 1661 (amide C=O) cm-1.

57184-25-5, 57184-25-5 1-(Cyclopropylmethyl)piperazine 965875, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Ebdrup, Soren; de Jong, Johannes Cornelis; Jacobsen, Poul; Hansen, Holger Claus; Vedso, Per; US2003/166644; (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.196811-66-2,tert-Butyl 4-carbamothioylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

To a stirred solution of tert-butyl 4-carbamothioylpiperazine-1-carboxylate (synthesized according to Example 5, Step 1, 2.0 g, 8.16 mmol) in dioxane (20 mL), TEA (1.7 mL, 10.6 mmol) and 1-bromobutan-2-one (1.2 mL, 10 mmol) were added and stirred at 80 C for 16 h. The completion of the reaction was monitored by TLC. The reaction mixture was quenched with water (10 mL) and extracted with EtOAc (2 x 25 mL). The organic layer was separated, dried over anhydrous Na2SO4, concentrated under vacuum. The resulting product was taken as such for next step. Yield: 86% (2.1 g, pale yellow solid). LCMS: (Method A) 298.0 (M+H), Rt. 2.94 min, 93.1 % (Max)., 196811-66-2

196811-66-2 tert-Butyl 4-carbamothioylpiperazine-1-carboxylate 12093220, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; ASCENEURON SA; QUATTROPANI, Anna; KULKARNI, Santosh S.; GIRI, Awadut Gajendra; (243 pag.)WO2016/30443; (2016); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics