Category: 5625-67-2

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, EXAMPLE 151 EPO Preparation of 4-(4-methyl-2-piperazinon- 1 -yl)piperidin- 1 -yl-2-(2-methoxyphenyl)-2-(4- chlorophenylaminocarbonylamino)-acetamide; A. Preparation of 4-(4-methyl-2-piperazinon-l-yl)piperidine; [0523] To a solution of 2-pirhoerazinone (200 mg, 2.00 nimol) and HCHO (37% aq., 0.200 mL, 2.69 mmol) in MeOH (6 niL) at room temperature, NaBH3CN (162 mg, 2.57 mmol) was added. After being stirred at room temperature overnight, the solution was concentrated in vacuo. The residue was partitioned between 5% aq. NaHCO3 and nBuOH. The nBuOH phase was separated, concentrated in vacuo to give the 4-methyl-2-piperazinone as a semi-solid (118 mg). MS 115.5 (M+H).[0524] A mixture of 4-iodopyridine (218 mg, 1.06 mmol), 4-methyl-2-piperazinone (106 mg, 0.929 mmol), K3PO4 (425 mg, 2.00 mmol) and 1,2-trans-diaminocyclohexane (0.050 mL, 0.41 mmol) in anhydrous dioxane (3.0 mL) was degassed with Ar before being charged with CuI (40 mg, 0.21 mmol). The mixture in a sealed tube was heated at 1100C overnight. The mixture was purified by a prep-TLC using MeOHZCH2Cl2 (10/90) as solvents to give 1- (pyridin-4-yl)-4-methyl-2-piperazinone (42 mg). MS 192.5 (M+H).[0525] A mixture of l-(pyridin-4-yl)-4-methyl-2-piperazinone (12 mg, 0.063 mmol) and PtO2 (49 mg) in HOAc (6.0 mL) was hydrogenated on a Parr shaker under 40 psi for 3 days. The mixture was filtered through celite. The filtrate was concentrated in vacuo. The residue was dissolved in IN HCl (5.0 mL). The solution was then concentrated in vacuo to give the titled compound as hydrochloride salt (12 mg). MS 198.5 (M+H).

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

Reference：
Patent; PORTOLA PHARMACEUTICALS, INC.; WO2006/63113; (2006); A2;,
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

To a mixture of piperazine-2-one (1.037 g, 10.4 mmol) in 52 mL of CH2Cl2, was added BOC20 (2.5 g, 11.4 mmol). The reaction became homogeneous after 3 hours when the starting material was completely consumed. The reaction was diluted with CH2Cl2 and the organic layer was washed with water. The solvent was removed in vacuo to yield quantitative amount of product 33 as a white solid. ?H NMR (300 MHz, CDCl3) 8 1.48 (s, 9H), 3.35-3.44 (m, 2H), 3.64 (t, 2H, J= 5 Hz), 4.10 (s, 2H), 6.41 (br s, 1H).

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

Reference：
Patent; GILEAD SCIENCES, INC.; CAI, Zhenhong, R.; CHEN, Xiaowu; FARDIS, Maria; JABRI, Salman, Y.; JIN, Haolun; KIM, Choung, U.; METOBO, Sanuel, E.; MISH, Michael, R.; PASTOR, Richard, M.; WO2005/117904; (2005); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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.

iii 3-Oxo-piperazine-1-carboxylic Acid Tert-Butyl Ester Oxopiperazine (3.38 g, 34 mmol) is dissolved in 20 mL of CH2Cl2. Et3N (9.5 mL, 68 mmol) is added followed by Boc2O (7.4 g, 34 mmol). The solution is allowed to stir at ambient temperature for 3 hours, at which time the reaction is quenched by the addition of brine. The phases are separated and the organic phase is washed with brine, 1 M aqueous KH2PO4 and dried over Na2SO4. The mixture is filtered and concentrated to give iii as a white solid (6.1 g, 30 mmol, 90%). (MS: M+H: 199.0).

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

Reference：
Patent; Gailunas, Andrea; Tucker, John A.; TenBrink, Ruth; Mickelson, John; US2003/109559; (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.5625-67-2,Piperazin-2-one,as a common compound, the synthetic route is as follows.

5625-67-2, Di-tert-butyl dicarbonate (3.92 g, 17.98 mmol) was added to a suspension of 2-piperazinone (1.50 g, 14.98 mmol) in dichloromethane (15 mL). The mixture was stirred at room temperature for 5 hours. The solvent was evaporated to afford 1 ,1- dimethylethyl 3-oxo-1-piperazinecarboxylate (2.99 g, quantitative) as an off-white solid.

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

Reference£º
Patent; GLAXOSMITHKLINE LLC; BANKA, Anna; CATALANO, John, G.; CHONG, Pek, Yoke; FANG, Jing; GARRIDO, Dulce, Maria; PEAT, Andrew, James; PRICE, Daniel, J.; SHOTWELL, John, Brad; TAI, Vincent; ZHANG, Huichang; WO2011/41713; (2011); A2;,
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

A 2-l Erlenmeyer flask was charged with 2-piperazinone (36.5 g, 364 mmol), sodium carbonate (116 g, 1.10 mol), 600 ml dioxane, and 150 ml water at room temperature. To this was slowly added benzyl chloroformate (62.1 g,364 mmol) over 20 min. After the addition was complete, the mixture was stirred for 2 h, diluted with water and extracted with 2 l of ethyl acetate. The combined organic extracts were dried (MgSO4), filtered and concentrated to give a white solid.To this solid was added 500 ml CH2Cl2, triethylamine (92.6 g, 128 ml, 911 mmol), 4-dimethylaminopyridine (4.45 g, 36.4 mmol), and di-tert-butyl dicarbonate (119 g,546 mmol). After 1 h at room temperature, the mixture was diluted with water and the organics were separated, dried (MgSO4), filtered and concentrated to give a brown oil. To this oil was added 100 ml CH2Cl2 followed by 1 l hexane. The resulting white solid was collected by filtration to give 4-benzyl 1-tert-butyl 2-oxo-1,4-piperazinedicarboxylate (101 g, 81%). 1H-NMR (400 MHz, CDCl3) delta 7.45-7.29 (m, 5 H), 5.15 (s, 2H), 4.24 (s, 2 H), 3.88-3.74 (m, 2 H), 3.74-3.59 (m, 2 H), 1.54 (s, 9H).

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

Reference£º
Article; Lloyd, David J.; St Jean, David J.; Kurzeja, Robert J. M.; Wahl, Robert C.; Michelsen, Klaus; Cupples, Rod; Chen, Michelle; Wu, John; Sivits, Glenn; Helmering, Joan; Komorowski, Renee; Ashton, Kate S.; Pennington, Lewis D.; Fotsch, Christopher; Vazir, Mukta; Chen, Kui; Chmait, Samer; Zhang, Jiandong; Liu, Longbin; Norman, Mark H.; Andrews, Kristin L.; Bartberger, Michael D.; Van, Gwyneth; Galbreath, Elizabeth J.; Vonderfecht, Steven L.; Wang, Minghan; Jordan, Steven R.; Veniant, Murielle M.; Hale, Clarence; Nature; vol. 504; 7480; (2013); p. 437 – 440;,
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, Step 1 tert-butyl 4-benzyl-3-oxopiperazine-1-carboxylate Di-tert-butyl dicarbonate (750 mg, 3.44 mmol) was added to a solution of piperazine-2-one (344 mg, 3.44 mmol) in CH2Cl2 (13 mL). The solution was stirred at room temperature for 16 hours, then concentrated under vacuum. The residue was dissolved in N,N-dimethylformamide (10 mL) and stirred under nitrogen as sodium hydride (60% dispersion in oil, 0.25 g, 6.25 mmol) was added at room temperature. The mixture was stirred for 30 minutes, then benzyl bromide (0.532 mL, 4.47 mmol) was added. The mixture was stirred under nitrogen for 1 hour, and the reaction was quenched by cautious addition of water (3 mL). Finally, the mixture was diluted with water (50 mL) and stirred at room temperature for 2 hours. The resulting precipitate was collected by filtration and washed with water (40 mL), then dried under vacuum to the titled compound (0.82 g, 82%). 1H NMR (400 MHz, methanol-d4) delta ppm 1.46 (s, 9H), 3.30-3.33 (m, 2H), 3.60 (t, J=5.2 Hz, 2H), 4.11 (s, 2H), 4.62 (s, 2H), 7.25-7.37 (m, 5H); MS (ESI) m/z 291 (M+H)+.

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

Reference£º
Patent; ABBVIE INC.; Bunnelle, William; Cowart, Marlon; Drizin, Irene; Koenig, John Robert; Pliushchev, Marina; Scanio, Marc; (80 pag.)US2016/376240; (2016); 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, Piperazine -2-one( 2g, 20 mmol) is added to DCM (30 mL) ,and under the protection of argon Et3N (3.46 mL, 24 mmol) is added ,after cooling down the room temperature to 0 , add BOC anhydride (4.79g, 22mmol) in one reaction flask and raise the room temperature . After 3 h, reaction is stopped and DCM (100 mL) is added, washed with saturated NaCl solution (30 mL x 2), dried over anhydrous magnesium sulfate, concentrated, and recrystallized from DCM and petroleum ether to give a white solid 2.8 g, yield 70%.

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

Reference£º
Patent; Chinese Academy Of Medical Sciences Pharmaceutical Institute; Xu Boling; Chen Xiaoguang; Zhou Jie; Ji Ming; Yao Haiping; Zhou Qin; (57 pag.)CN107098886; (2017); A;,
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

Piperazine-2-one (1.0 g, 10 mmol) was suspended in 10 mL DCM and Boc2O was slowly added. After the addition was completed, it was allowed to stand overnight at room temperature.After completion of the reaction, it was washed three times with 0.1 N diluted hydrochloric acid, 20 ml each time, and washed three times with 20 ml of saturated potassium carbonate each time.Finally, the dichloromethane was dried over anhydrous sodium sulfate.The solution was removed under vacuum to give a white solid.

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

Reference£º
Patent; Shaoxing University; Hu Chunqi; Li Xin; Shi Yaru; Du Wenting; Tong Jie; Su Wanting; Xia Weiqi; (20 pag.)CN108610332; (2018); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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.

To a solution of piperazinone (10.0 g, 100 mmol), Triethylamine (20.2 g, 200mmol), and DMAP (50 mg) in CHaCIa (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 (MgSO4) andconcentrated to give the product (18.0 g, 90%). MS m/e 201 (M+H)”1″

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

Reference£º
Patent; SCHERING CORPORATION; WO2006/14944; (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

The 1-(4-fluorophenyl)-2-piperazinone used in the above procedure was prepared as follows:A mixture of 2-piperazinone (1.5 g, 15.0 mmol), 1-fluoro-4-iodobenzene (3.5 ml, 30.0 mmol), copper(l) iodide (0.57 g, 3.0 mmol), N,N’-dimethyl-1 ,2-cyclohexanediamine (0.95 ml, 6.0 mmol) and potassium phosphate (9.5 g, 44.9 mmol) in 1 ,4-dioxane (20 ml) was heated at reflux (1 10 0C) under argon for 24 hours. The mixture was allowed to cool to room temperature and then diluted with methanol, and filtered through a pad of celite, washing with methanol. The filtrate was evaporated in vacuo and the resulting residue was dissolved in dichloromethane and 0.88 aqueous ammonia solution (~5ml) in water (~30ml). The mixture was then extracted into dichloromethane (x3), and the combined organic extracts were washed with water (x1 ) and dried over magnesium sulphate. The solvent was evaporated in vacuo and the crude product was purified further by column chromatography on flash-silica gel, eluting with 0-10percent methanol in dichloromethane. The relevant fractions were combined and the solvent was evaporated in vacuo. The residue was purified by SCX, eluting first with methanol and then with 2M ammonia in methanol. The basic fractions were combined and the solvent was evaporated in vacuo to give crude product which was purified again by flash-silica gel column chromatography, eluting with 20percent 2M ammonia in methanol in dichloromethane, to give 1-(4-fluorophenyl)-2- piperazinone (560 mg) as a colourless solid. LC/MS [M+H]+ = 195., 5625-67-2

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

Reference£º
Patent; GLAXO GROUP LIMITED; WO2009/53459; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics