Month: December 2020

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4318-42-7,1-Isopropylpiperazine,as a common compound, the synthetic route is as follows.,4318-42-7

Preparation 15: 4-(4-i-Propylpiperazin-l-yl)cyclohexanamine (cis and trans isomers); [0124] In a 250 mL flask, 4-acetamidocyclohexanone (4 g, 25.8 mmol), N-i-propyl piperazine (6 g, 46.9 mmol) were dissolved in dry toluene (125 mL) and added methanesulfonic acid (MSA) (1 mL) and refluxed using Dean-Stark apparatus for five hours with occasional decanting toluene from Dean-Stark apparatus 3-4 times. Then removed half of the toluene from the apparatus and cooled to 500C and added 75 mL ethanol then removed the Dean-Stark apparatus and cooled to 15-200C. Added NaBH4 (35.4 mmol) portion wise under nitrogen atmosphere. Continued stirring the reaction for overnight. After 30 min 20 mL of 4 N HCl was added drop wise to the reaction. The volatiles removed from the reaction under reduced pressure. Basified the gummy solid reaction mixture with 20 mL sat. K2CO3, diluted with another 20 mL water and further basified with 50percent NaOH solution to pH about 13. Then added EtOAc (100 mL) and filtered the solid product and washed with EtOAc and ether and collected cyclohexanamine N-(4-(4-i-propylpiperazin-l-yl)cyclohexyl)acetamide (cis and trans isomers) as white powder (5.2 g, 75.6percent). ESI-MS: m/z 268 (M+H) +. N-(4-(4- propylpiperazin-l-yl)cyclohexyl)acetamide (5.2 g, 19.5 mmol) was refluxed in 24percent cone. HCl solution for 20 hours at 115¡ãC. Then evaporated the solution under reduced pressure and the solid product obtained was dissolved and recrystallized from isopropyl alcohol to get the product as white hydrochloride salt (6.7 g). ESI-MS: m/z 226 (M+H)+.

As the paragraph descriping shows that 4318-42-7 is playing an increasingly important role.

Reference£º
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; CAO, Sheldon X.; ICHIKAWA, Takashi; KIRYANOV, Andre, A.; MCBRIDE, Christopher; NATALA, Srinivasa, Reddy; KALDOR, Stephen, W.; STAFFORD, Jeffrey, A.; WO2010/25073; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

163765-44-4, (R)-1-Boc-3-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step 2: (R)-tert-Butyl 3-methyl-4-(3-(methylcarbamoyl)pyridin-2-yl)piperazine-1-carboxylate At rt, to a solution of 2-chloro-N-methyl-pyridine-3-carboxamide (300.00 mg, 1.76 mmol) in DMF (8.00 mL) was added (R)-tert-butyl 3-methylpiperazine-1-carboxylate (1.06 g, 5.28 mmol) and K2CO3 (729.75 mg, 5.28 mmol). The reaction mixture was stirred at 130 C. for 4 h under microwave. Then cooled to rt and diluted with H2O (100 mL), extracted with EtOAc (60 mL*3), the combined organic layer was washed with brine, dried (Na2SO4), filtered, concentrated and purified by chromatography (silica, ethyl acetate/petroleum ether=1/5) to afford (R)-tert-butyl 3-methyl-4-(3-(methylcarbamoyl)pyridin-2-yl)piperazine-1-carboxylate (450.00 mg, 1.35 mmol, 76.70% yield) as solid. ESI-MS (EI+, m/z): 335.0 [M+H]+, 163765-44-4

As the paragraph descriping shows that 163765-44-4 is playing an increasingly important role.

Reference£º
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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5308-25-8,1-Ethylpiperazine,as a common compound, the synthetic route is as follows.

5308-25-8, General procedure: A solution of compound 2 (0.55 mmol), 1-substituted piperazine (0.83 mmol) and pyridine (0.8 mmol) in 10 mL THF (tetrahydrofuran) was stirred at room temperature overnight. When the reaction was completed, the solvent was evaporated under reduced pressure. The residues were dissolved in ethyl acetate and washed with water and saturated sodium chloride solution. After drying over anhydrous Na2SO4, the solvent was removed under reduced pressure to get crude product. The pure products were obtained by recrystallizing from ethanol.

5308-25-8 1-Ethylpiperazine 79196, apiperazines compound, is more and more widely used in various fields.

Reference£º
Article; Wu, Zhilin; Ding, Na; Tang, Yuting; Ye, Jiao; Peng, Junmei; Hu, Aixi; Research on Chemical Intermediates; vol. 43; 8; (2017); p. 4833 – 4850;,
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.21655-48-1,cis-2,6-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

Intermediate 21: Ethyl 4-{cis-3,5-dimethyl-(piperazin-1-yl)}-benzoate Dimethyl sulfoxide (10 ml) was added to 3.6 g of cis-2,6-dimethylpiperazine to prepare a suspension, and 2.5 g of ethyl 4-fluorobenzoate was added to the suspension. The mixture was stirred at 80 C. for 24 hr and was then cooled to room temperature, and 100 mg of water was added thereto. The mixture was extracted three times with 100 ml of ethyl acetate. The combined organic layer was dried over anhydrous magnesium sulfate, and concentrated under the reduced pressure. The residue was purified by column chromatography on silica gel (development system: methylene chloride-methanol-concentrated aqueous ammonia=900:100:1) to prepare 1.5 g of the title compound. Physicochemical Properties of Intermediate 21, 21655-48-1

21655-48-1 cis-2,6-Dimethylpiperazine 6950261, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Meiji Seika Kaisha, Ltd.; US6451800; (2002); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

13484-40-7, 1-(2-Methoxyethyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Compound 27 (prepared according to B 15) (0.133 g; 0.0002 mol) was dissolved in DMF (2 ml). PS-CDI, 1.9 mmol/g (0.320 g; 0.0006 mol) was added and HOBT (0.041 g; 0.003 mol) in DMF (2 ml) was added. The reaction mixture was shaken for 1 hour at room temperature. l-(2-Methoxyethyl)piperazine (0.0002 mol) in DMF (2 ml) was added. The reaction mixture was shaken overnight. MP-carbonate, 1 mmol/g (0.5 g) and polymer-bound isocyanate (0.111 g; 0.0002 mol) were added. The reaction mixture was shaken overnight. The reaction mixture was filtered, CH2Cl2 (3 ml) was added, and the mixture was shaken for 2 hours and filtered again. The filtrate was evaporated with the Genevac. The product was purified by reversed-phase high-performance liquid chromatography (Shandon Hyperprep C 18 BDS (Base Deactivated Silica) 8 mum, 250 g, LD. 5 cm). A gradient with 3 mobile phases was applied. Phase A: a 0.25 % NH4HCO3 solution in water; phase B : CH3OH; phase C: CH3CN). The desired fractions were collected and the solvent was evaporated. Yield: 22 mg of compound 275.

13484-40-7, 13484-40-7 1-(2-Methoxyethyl)piperazine 2734638, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; JANSSEN PHARMACEUTICA N.V.; WO2008/148868; (2008); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

163765-44-4, (R)-1-Boc-3-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Intermediate 34: (2R)-2-methyl-1-(methylsulfonyl)piperazine hydrochloride; To a solution of 1 , 1-dimethylethyl (3R)-3-methyl-1-piperazinecarboxylate(commercially available, for example from Sigma Aldrich, St Louis, USA, 1 .18 g, 4.98 mmol) in NaOH (2 M aqueous) (6.23 ml, 12.5 mmol) and THF (10 ml) at rt was added mesyl chloride (0.408 ml, 5.23 mmol) over 30 seconds. The solution was stirredvigorously at rt for 2 hours. Additional mesyl chloride (0.408 ml, 5.23 mmol) wasadded and the reaction was stirred vigorously at rt for 2 hours. Additional mesyl chloride (0.408 ml, 5.23 mmol) was added and the solution stirred vigorously at rt for 18 hours. The reaction was diluted with ethyl acetate (50 ml), then washed with 2M aqueous HCI (2 x 25 ml), brine (25 ml), dried (MgS04), filtered and concentrated under vacuum to leave a clear oil (900 mg) that became a crystalline white solid on standing overnight. This was redissolved in DCM (5.0 ml), then TFA (1.24 ml, 16.2 mmol) was added and the solution heated at reflux for 2 hours. The solution was cooled to rt, and concentrated under vacuum to leave a pale orange paste. This was re-dissolved in methanol (10 ml) and applied to an SCX-2 cartridge (25 g), washing with MeOH (50 ml). The product was eluted with 2M NH3 in MeOH (50 ml) and the solvent removed under vacuum to leave a viscous clear oil (361 mg). This was re- dissolved in methanol (10 ml) and aqueous HCI (2 M, 2.0 ml, 4.00 mmol) added. Concentration under vacuum, followed by azeotroping with toluene (2 x 25 ml) left a white solid, (2R)-2-methyl-1 -(methylsulfonyl)piperazine hydrochloride (412 mg).1H NMR (400 MHz, DMSO-d6) delta ppm 1 .35 (d, J=7.0 Hz, 3 H), 2 91 (m, 1 H), 3.04 (s, 3 H), 3.06 – 3.21 (m, 3 H), 3.33 (ddd, J=14.5, 12.1 , 2.9 Hz, 1 H), 3.61 (d, J=14. 5 Hz, 1 H), 4.13 (m, 1 H), 9.26 (br s, 1 H), 9.83 (br s, 1 H).

163765-44-4, 163765-44-4 (R)-1-Boc-3-Methylpiperazine 2756811, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; CONVERGENCE PHARMACEUTICALS LIMITED; BESWICK, Paul John; GLEAVE, Robert James; HACHISU, Shuji; VILE, Sadie; BERTHELEME, Nicolas; WARD, Simon E; WO2012/4604; (2012); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

31.5 g of 4-chloro-1-nitrobenzene and 44.4 ml of 1-methyl-piperazine are combined and stirred for 18 hours at 90 C. Then the solution is poured onto ice water and the precipitate formed is suction filtered, washed with water and recrystallised from ethanol/water (1:1). The residue is dried in vacuo at 75 C. [00369] Yield: 44.0 g (99% of theory), [00370] Rf value: 0.5 (silica gel, methylene chloride/methanol=10:1) [00371] Melting point: 108-112 C., 109-01-3

The synthetic route of 109-01-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Boehringer Ingelheim Pharma GmbH & Co. KG; US6794395; (2004); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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

Step 2: A mixture of 0.2 g (0.50 mmol) intermediate II.5 step 1 , 70 mg (0.61 mmol) 1 – Methylpiperazin-2-one, 90 mg (0.65 mmol) K2C03 and acetonitrile is heated to 80¡ãC in a pressure tube for 3.5 h. After cooling to RT the solvent is evaporated and DCM and water are added. The organic phase is separated, dried, filtered and evaporated. (0548) Yield: 0.1 g (Yield 59percent), ESI-MS: m/z = 436 M+H+, R,(HPLC) : 0.25 min (HPLC-W), 59702-07-7

As the paragraph descriping shows that 59702-07-7 is playing an increasingly important role.

Reference£º
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BLUM, Andreas; WO2015/169677; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5308-25-8, 1-Ethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5308-25-8, Step 7: 1-ethyl-4-(5-nitropyridin-2-yl)piperazine 2-Chloro-5-nitropyridine (800 mg, 5.05 mmol) was dissolved in dioxane (20 mL) and then 1-ethylpiperazine (1.7 g, 15.15 mmol) and N,N-diisopropylethylamine (927 mL, 5.05 mmol) were added. The reaction mixture solution was stirred at 70 C. for a day. The reaction solution was cooled to room temperature, diluted with ethyl acetate, and then washed with brine. The organic layer was concentrated by drying with magnesium sulfate. The target compound (1.05 g, 87% yield) was used in the following reaction without purification. MS m/z: 237.51 [M+1].

5308-25-8 1-Ethylpiperazine 79196, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Sim, Tae Bo; Hah, Jung Mi; Choi, Hwan Geun; Ham, Young Jin; Lee, Jung Hun; Park, Dong Sik; Kim, Hwan; US2013/12703; (2013); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

76003-29-7,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.76003-29-7,1-Boc-3-Oxopiperazine,as a common compound, the synthetic route is as follows.

A 60% dispersion of sodium hydride in mineral oil (3.6 g, 150 mmol, 1.5 equiv) was added in portions to a solution of tert- butyl 3-oxopiperazine-l-carboxylate (20.02 g, 100 mmol, 1 equiv) in anhydrous THF (400 mL) at 5 C and the mixture was stirred at room temperature for 1.5 hours. Benzyl bromide (14.27 mL, 120 mmol, 1.2 equiv) was added and the mixture was stirred at room temperature for 15 hours. Water (100 mL) was carefully added to quench the reaction and the mixture was extracted with ethyl acetate (3 x 200 mL). The combined organic layers were washed with saturated brine (200 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was triturated with heptanes (200 mL) to give tert-butyl 4-benzyl-3-oxopiperazine-l- carboxylate (23.5 g, 81% yield) as a white solid.

The synthetic route of 76003-29-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; CONATUS PHARMACEUTICALS, INC.; SPADA, Alfred, P.; TERNANSKY, Robert, J.; (0 pag.)WO2020/6341; (2020); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics