Category: 5625-67-2

5625-67-2,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5625-67-2,Piperazin-2-one,as a common compound, the synthetic route is as follows.

A 2-L Erlenmeyer flask was charged with 2-piperazinone (36.5 g, 364 mmol, Sigma- Aldrich, St. Louis, MO), sodium carbonate (116 g, 1093 mmol), 600 mL of dioxane, and 150 mL of water. To this was slowly added benzyl chloroformate (62.1 g, 364 mmol, Sigma-Aldrich, St. Louis, MO) at room temperature over 20 min. After the addition was complete, the mixture was stirred for 2 h and then diluted with water and extracted with EtOAc (2 L). The combined organic extracts were dried (MgS04), filtered, and concentrated to give a white solid. To this solid was added 500 mL of DCM, triethylamine (128 mL, 911 mmol), DMAP (4.45 g, 36.4 mmol), and di-tert-butyl dicarbonate (119 g, 546 mmol, Sigma-Aldrich, St. Louis, MO). After 1 h at room temperature, the mixture was diluted with water and the organics were separated. The organics were dried (MgS04), filtered, and concentrated to give a brown oil. To this oil was added 100 mL of DCM followed by 1 L of hexane. The resulting white solid was collected by filtration to give 4-benzyl 1-tert-butyl 2-oxo-l,4- piperazinedicarboxylate (101 g).

The synthetic route of 5625-67-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; AMGEN INC.; ASHTON, Kate; BARTBERGER, Michael David; BO, Yunxin; BRYAN, Marian C.; CROGHAN, Michael; FOTSCH, Christopher Harold; HALE, Clarence Henderson; KUNZ, Roxanne Kay; LIU, Longbin; NISHIMURA, Nobuko; NORMAN, Mark H.; PENNINGTON, Lewis Dale; POON, Steve Fong; STEC, Markian Myroslaw; ST. JEAN, David, Joseph, Jr.; TAMAYO, Nuria A.; TEGLEY, Christopher Michael; YANG, Kevin Chao; WO2012/27261; (2012); 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.5625-67-2,Piperazin-2-one,as a common compound, the synthetic route is as follows.

5625-67-2, Step 2 benzyl 3-oxopiperazine-1-carboxylate At 0C, to a mixture solution of sodium carbonate (24.77 g, 233.73 mmol, 3.00 equivalents) and piperazine-2-one (7.80 g, 77.91 mmol, 1.00 equivalent) in ethyl acetate (70.00 mL) and water (70.00 mL) was added benzyl chloroformate (16.79 g, 93.49 mmol, 13.99 mL, 95% purity, 1.20 equivalents). The reaction mixture was stirred at 30C for 16 hours. TLC showed completiton of the reaction. The mixture was subjected to extraction using ethyl acetate (80 mL*3). The combined organic layers was washed with a saturated aqueous solution of sodium chloride (80 mL*3), dried over sodium sulfate and concentrated in vacuo to give a crude product. The crude product was beaten in (petroleum ether: ethyl acetate = 20: I, 80 mL). The resulting mixture was stirred at 30C for 15 minutes and filtered. The solid was dried in vacuo to give the title compound (15.50 g, 66.17 mmol, 84.93% yield) as a white solid.

The synthetic route of 5625-67-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Chai Tai Tianqing Pharmaceutical Group Co., Ltd.; Medshine Discovery Inc.; DING, Charles Z.; CHEN, Shuhui; ZHAO, Baoping; XU, Zhaobing; LIU, Yingchun; LIN, Ruibin; WANG, Fei; LI, Jian; (101 pag.)EP3269715; (2018); 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.5625-67-2,Piperazin-2-one,as a common compound, the synthetic route is as follows.

A 2-L Erlenmeyer flask was charged with 2-piperazinone (36.5 g, 364 mmol, Sigma-Aldrich, St. Louis, MO), sodium carbonate (116 g, 1090 mmol, J. T. Baker, Philipsburg, NJ), 600 mL of dioxane, and 150 mL of water. To this was slowly added benzyl chloroformate (62.1 g, 364 mmol, Sigma-Aldrich, St. Louis, MO) at rt over 20 min. After the addition was complete, the mixture was stirred for 2 h and then diluted with water and extracted with EtOAc (2 L). The combined organic extracts were dried (MgS04), filtered, and concentrated to give a white solid. To this solid was added 500 mL of DCM, triethylamine (128 mL, 911 mmol, Sigma-Aldrich, St. Louis, MO), DMAP (4.45 g, 36.4 mmol, Sigma- Aldrich, St. Louis, MO), and di-tert-butyl dicarbonate (119 g, 546 mmol, Sigma- Aldrich, St. Louis, MO). After stirring at room temperature for 1 h, the mixture was diluted with water and the organics were separated. The organics were dried (MgS04), filtered, and concentrated to give a brown oil. To this oil was added 100 mL of DCM followed by 1 L of hexane. The resulting white solid was collected by filtration to give 4-benzyl 1-tert-butyl 2-oxo-l,4- piperazinedicarboxylate (101 g)., 5625-67-2

As the paragraph descriping shows that 5625-67-2 is playing an increasingly important role.

Reference£º
Patent; AMGEN INC.; ASHTON, Kate; FOTSCH, Christopher H.; KUNZ, Roxanne K.; LIU, Longbin; NISHIMURA, Nobuko; NORMAN, Mark H.; SIEGMUND, Aaron C.; ST. JEAN, JR., David J.; TAMAYO, Nuria A.; YANG, Kevin C.; WO2014/35872; (2014); 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.5625-67-2,Piperazin-2-one,as a common compound, the synthetic route is as follows.

5625-67-2, 1) 3-Oxopiperazine-1-carboxylic acid tert-butyl ester Triethylamine (3.83 mL) and di-tert-butoxydicarbonate (6.32 mL) were added at room temperature to piperazin-2-one (2.5 g) in a mixture of tetrahydrofuran (50 mL) and methanol (50 mL), followed by stirring for 4 hours. The reaction solvent was evaporated under reduced pressure. The residue was partitioned between water and ethyl acetate. The organic layer was sequentially washed with water and saturated brine. The aqueous layers obtained through washing were combined, and the combined layer was extracted with ethyl acetate. The organic layers were combined, followed by drying over magnesium sulfate anhydrate. After a filtration step, the solvent was evaporated under reduced pressure. Subsequently, ethyl acetate-hexane was added to the residue, followed by drying to solid, to thereby give 3-oxopiperazine-1-carboxylic acid tert-butyl ester (3.6 g, 72%). 1H-NMR(400MHz,CDCl3)delta:1.48(9H,s), 3.37-3.40(2H,m), 3.62-3.65(2H,m), 4.01(2H,s), 6.32(1H,br s). [Referential Example 40] 1-Ethyl-2-oxopiperazine hydrochloride [Show Image] 1) 3-Oxopiperazine-1-carboxylic acid tert-butyl ester Piperazin-2-one (5.07 g) was dissolved in tetrahydrofuran (50 mL) and methanol (50 mL), and, at room temperature, triethylamine (7.76 mL) and di-tert-butyl dicarbonate (12.17 g) were added to the solution, followed by stirring for 4 hours. The reaction solvent was evaporated under reduced pressure, and diethyl ether was added to the residue. The precipitated solid was collected through filtration, to thereby give 3-oxopiperazine-1-carboxylic acid tert-butyl ester as a solid product (9.36 g, 92%). 1H-NMR(400MHz,DMSO-d6)delta:1.40(9H,s), 3.15(2H,br), 3.45(2H,br), 3.81(2H,br), 8.03(1H,br). ESI-MS m/z:201(M+H)+.

As the paragraph descriping shows that 5625-67-2 is playing an increasingly important role.

Reference£º
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1762568; (2007); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5625-67-2, Piperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5625-67-2, To a solution of piperazinone (10.0 g, 100 mmol), triethylamine (20.2 g, 200mmol), and DMAP (50 mg) in CH2CI2 (250 ml) in an ice-water bath was added(Boc)2O (22.9 g, 105 mmol) slowly. The mixture was stirred in the ice-water bath for 1h and at RT for 4.5 h. The mixture was diluted with CH2CI2 (250 ml), washed withwater (200 ml), 5% citric acid (200 ml), 1N HCI (200 ml), saturated sodiumbicarbonate (20 ml) and brine. The organic layer was dried (MgSCU) andconcentrated to give the product (18.0 g, 90%). MS m/e 201 (M+H)+

5625-67-2 Piperazin-2-one 231360, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; SCHERING CORPORATION; WO2006/14762; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5625-67-2, Piperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5625-67-2, Boc2O (2.0 mmol, 436mg, 1.0 eq) was added in portions under stirring and cooling on an ice bath to a suspension of piperazin-2-one (2.0 mmol, 200 mg, 1.0 eq) in anhydrous dichloromethane (10.0 mL). The reaction mixture was stirred overnight at room temperature, during which a homogeneous solutionformed. The solvent was evaporated and the solid residue was vacuum-dried tofurnish a yellow solid (300.0 mg, 100%). 1H NMR (300 MHz, CDCl3) delta (ppm): 1.51(s, 9 H); 3.37-3.46 (m, 2 H); 3.66 (t, J= 5.2 Hz, 2 H); 4.12 (s, 2 H); 6.39 (bs, 1 H). 13C NMR (75 MHz, CDCl3) delta (ppm):27.4 (CH2); 28.3 (3 x CH3); 41.2 (CH2); 77.1(CH2); 80.9 (C); 153.9 (C); 168.0 (C). MS (DCI/NH3) m/z: 201.1 [M+H+]; 218.1 [M + NH4+].

The synthetic route of 5625-67-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Chollet, Aurelien; Mori, Giorgia; Menendez, Christophe; Rodriguez, Frederic; Fabing, Isabelle; Pasca, Maria Rosalia; Madacki, Jan; Kordulakova, Jana; Constant, Patricia; Quemard, Annaik; Bernardes-Genisson, Vania; Lherbet, Christian; Baltas, Michel; European Journal of Medicinal Chemistry; vol. 101; (2015); p. 218 – 235;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics