Category: 109-07-9

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

Reference Example 2 Synthesis of t-butyl 3-methylpiperazine-1-carboxylate Under ice-cooling, 15 ml of tetrahydrofuran (THF) solution containing 10.9 g of DIBOC was added to 150 ml of THF solution containing 10 g of 2-methylpiperazine.. After stirring overnight, the solvent was evaporated under reduced pressure.. The residue was mixed with water and extracted with ethyl acetate, and then the organic layer was washed and dried and the solvent was evaporated under reduced pressure to obtain 8.94 g of the title compound as a yellow oily substance.

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

Reference£º
Patent; Yamanouchi Pharmaceutical Co. Ltd.; US6673799; (2004); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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

EXAMPLE 7 1-Cyclopropyl-6-fluoro-1,4-dihydro-5-methyl-7-(3-methyl-1-piperazinyl)-4-oxo-3-quinolinecarboxylic acid A mixture of 0.75 g (2.68 mmol) of 1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-methyl-4-oxo-3-quinolinecarboxylic acid, 1.07 g (10.4 mmol) of 2-methylpiperazine and 30 ml of acetonitrile was refluxed for five hours, then stirred at room temperature overnight. The precipitate was filtered, washed with water/ethanol and acetonitrile, and dried to give 0.42 g of the title compound, mp 189-192 C., 109-07-9

The synthetic route of 109-07-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Warner-Lambert Company; US4920120; (1990); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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

Reference Example 10 Benzyl 3-methylpiperazine-1-carboxylate A 4 g portion of 2-methylpiperazine was dissolved in 40 ml of dichloromethane, and 1.71 g of benzyl chloroformate was added dropwise thereto at -78C. After 1 hour of stirring, the mixture was washed by adding water and dried and then the solvent was evaporated to obtain 2.0 g of the title compound., 109-07-9

109-07-9 2-Methylpiperazine 66057, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; YAMANOUCHI PHARMACEUTICAL CO. LTD.; EP1122242; (2001); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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

1) 3-Methylpiperazine-1-carboxylic acid tert-butyl ester Di-tert-butyl dicarbonate (21.7 g) was added at room temperature to 2-methylpiperazine (10.0 g) in methanol (200 mL), followed by stirring for 24 hours. The reaction solvent was removed under reduced pressure, and the residue was purified by silica gel column chromatography (chloroform – methanol), to thereby give 3-methylpiperazine-1-carboxylic acid tert-butyl ester as an oily product (19.3 g, 96.5percent). 1H-NMR (300MHz, CDCl3) delta: 1.04 (3H, d, J=6.24Hz), 1.46(9H,s), 2.39(1H,br s), 2.70-2.77(3H,m), 2.94(1H,br s), 3.93(2H,br s). MS(FAB)m/z:201(M+H)+.

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

Reference£º
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1621537; (2006); 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.109-07-9,2-Methylpiperazine,as a common compound, the synthetic route is as follows.

To a solution of 2-methylpiperazine (2.2 g) in tetrahydrofuran (15 ml) was added di-tert-butyl dicarbonate (4.0 g) slowly under ice-cooling, and the mixture was stirred at room temperature for 3.5 hours. Then the reaction mixture was diluted with ethyl acetate (20 ml), washed successively with water and brine, and dried over magnesium sulfate. The solvent was evaporated to give the title compound as a colorless oil. The obtained compound was used for the next step without further purification. [00318] 1H-NMR (300 MHz, CDCl3) delta 1.04 (d, J=5 Hz, 3H), 1.45 (s, 9H), 2.40 (br, 1H), 2.65-2.86 (m, 4H), 2.88-3.08 (m, 1H), 3.75-4.15(m, 2H).

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

Reference£º
Patent; Fujisawa Pharmaceutical Co., Ltd.; US6825200; (2004); B1;,
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.109-07-9,2-Methylpiperazine,as a common compound, the synthetic route is as follows.

Example 1: Ninety grams of L-CYCLOPROPYL-6, 7-DIFLUORO-1, 4-DIHYDRO-8-METHOXY-4-OXO-3- quinoline carboxylic acid and 64g (2.1 eq) of 2-methyl piperazine were put in suspension in 1.8 liter of DMSO under nitrogen atmosphere. The mixture was heated to 55 C during 24 hours. Subsequently, the mixture was heated to 70 C and half of the amount of DMSO was distilled-off at reduced pressure (1-5 mm Hg). At the end of the distillation, the reaction mixture was cooled to 20 C and left at this temperature overnight. The solution was then filtered under vacuum and the wet cake washed twice with n-butanol (300 ml). The collected solid was then dried under vacuum to obtain 94 g. The calculated yield, after assay, was 84%.

109-07-9, The synthetic route of 109-07-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; TEVA PHARMACEUTICAL INDUSTRIES LTD.; TEVA PHARMACEUTICALS USA, INC.; WO2004/69825; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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

To a solution of 2-methyl-piperazine (2.0 g, 0.02 mol) and triethylamine (6 mL) in methylene chloride (15 mL) at 0 C. was added (Boc)2O (4.14 g, 0.019 mol) dropwise. The mixture was stirred at room temperature for 1 hour, and then the solvent was removed by rotary evaporation. The residue was dissolved in methylene chloride, washed with saturated sodium bicarbonate and brine, dried over Na2SO4, and purified by column chromatography on silica gel (DCM:MeOH:Et3N=75:1:0.2) to give an white solid (1.65 g, 42%). LC-MS (ESI) m/z: 201 (M+1)+.

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

Reference£º
Patent; LEAD THERAPEUTICS, INC.; US2010/35883; (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.109-07-9,2-Methylpiperazine,as a common compound, the synthetic route is as follows.

Example 5 A reaction was carried out as described for Example 1, except that the solvent was changed from 44.7 g of 1-butanol to a mixed solvent consisting of 5.3 g of water and 40 g of 1-butanol (water content 10.6 wt%). After stirring at 0 to 5C for 2 hours, the reaction solution was analyzed. As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 82.1% (based on the amount of 2-methylpiperazine). Comparative Example 1 A reaction was carried out as described for Example 1, except that the solvent was changed from 44 g of 1-butanol to a mixed solvent consisting of 9 g of water and 35 g of 1-butanol (water content 20.5 wt%). After stirring at 0 to 5C for 2 hours, the reaction solution was analyzed. As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 59.6% (based on the amount of 2-methylpiperazine). Comparative Example 2 A reaction was carried out as described for Example 4, except that the solvent was changed from 44 g of 1-butanol to a mixed solvent consisting of 18 g of water and 27 g of 1-butanol (water content 40.0 wt%). After stirring at 0C for 2 hours, the reaction solution was analyzed. As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 51.6% (based on the amount of 2-methylpiperazine). Comparative Example 3 A reaction was carried out as described for Example 1, except that the solvent was changed from 44 g of 1-butanol to a mixed solvent consisting of 22 g of water and 22 g of 1-butanol (water content 50 wt%). After stirring at 0C for 2 hours, the reaction solution was analyzed. As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 33.6% (based on the amount of 2-methylpiperazine)., 109-07-9

109-07-9 2-Methylpiperazine 66057, apiperazines compound, is more and more widely used in various fields.

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

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

A mixture of 1-CYCLOPROPYL-6, 7-difluoro-1, 4-DIHYDRO-8-METHOXY-4-OXO-3- quinoline carboxylic acid (100G), 2-methylpiperazine (67.8gs) and anhydrous DMSO (300 ml) were stirred for 40-45 hrs at 60-65C. The reaction mass was then diluted with 1500 ml isopropyl alcohol. It was then stirred for 30 min at 25-30C followed by cooling at 5 to 10 C along with stirring for 2 hours. The product was obtained by filtration, which was washed with 3 x 50 ml isopropyl alcohol followed by drying at 50 to 55C for 4 hours to provide 71 g Gatifloxacin (Yield 55. 9%) Example 2: Step A: A mixture of L-CYCLOPROPYL-6, 7-difluoro-1, 4-dihydro-8-methoxy-4-oxo-3- quinoline carboxylic acid (120Kg) 2-methylpiperazine (40.8 Kg), and anhydrous DMSO (361 lit) was heated to 60-65C temperature and stirred for 2 hrs. A second lot of 2-methylpiperazine (10.2 Kg) was added, and stirred for next 1 hr, at 60-65C. followed by the addition of a third lot of 2-methylpiperazine (10.2Kg). The mixture was stirred for next 2 hrs at 60-65C. A fourth lot of 2-methylpiperazine (20.4Kg) was added to the mixture and the stirring was continued for the next 24 hrs maintaining the temperature at 60-65C followed by cooling to 25-35C. This reaction mass was added in 1802-1 isopropyl alcohol. Reaction mass was then stirred for 30 min at 25- 30C followed by cooling at 5 to 10 C along with stirring for 2 hours. Product so obtained was centrifuged, washed with 3 x 60-1 isopropyl alcohol. The wet cake of PRODUCT WAS MIXED WITH 241-LIT METHANOL AND STIRRED FOR 1 HR. , AGAIN THE PRODUCT WAS centrifuged followed by washing with 59 lit of methanol. The wet Gatifloxacin was dried at 60 to 65C for 6 hrs to yield 81. 92 Kg dry Gatifloxacin (Yield= 53.7%) HPLC Purity = 99.74% M/C=3. 42%, 109-07-9

109-07-9 2-Methylpiperazine 66057, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; CADILA HEALTHCARE LIMITED; WO2004/101527; (2004); 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.109-07-9,2-Methylpiperazine,as a common compound, the synthetic route is as follows.

Step 1: CbzCl (17 g, 0.1 mol) was added into a solution of compound 219-1 (30 g, 0.3 mol) and DIPEA (40 g, 0.3 mol) in DCM (200 mL) at 0C, then the mixture was stirred at room temperature for 3h and the solvent was removed, the crude product was purified by column chromatography to deliver compound 2 (11 g, yield 47%) as yellow oil. MS ESI calcd for C13H18N2O2 [M+H]+ 235, found 235., 109-07-9

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

Reference£º
Patent; GUANGDONG ZHONGSHENG PHARMACEUTICAL CO., LTD; WU, Hao; LIN, Jun; LI, Yunhui; WEI, Changqing; CHEN, Shuhui; LONG, Chaofeng; CHEN, Xiaoxin; LIU, Zhuowei; CHEN, Lijuan; (212 pag.)EP3124482; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics