Analyzing the synthesis route of 109-07-9

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

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.

Preparation of Benzoylpiperazine XXX To a stirred solution of 2-methylpiperazine (10.0 g, 0.1 mol) in dry CH2Cl2 (500 ml) under argon was added a solution of 1.0 M Me2AlCl or Et2AlCl in hexanes (100 ml, 0.1 mmol) and methyl benzoate (12.4 ml, 0.1 mmol) at room temperature. The reaction mixture was then stirred for 2 days before 2N NaOH (200 ml) was added. Aqueous layer was extracted with EtOAc (3*100 ml). The combined organic layer was dried over MgSO4 and concentration of solution provided 20.0 g of crude product (98%), with was pure enough for the further reactions., 109-07-9

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

Reference:
Patent; Bristol-Myers Squibb Company; US6469006; (2002); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 109-07-9

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

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.

Preparation of Benzoylpiperazine XXX To a stirred solution of 2-methylpiperazine (10.0 g, 0.1 mol) in dry CH2Cl2 (500 ml) under argon was added a solution of 1.0 M Me2AlCl or Et2AlCl in hexanes (100 ml, 0.1 mmol) and methyl benzoate (12.4 ml, 0.1 mmol) at room temperature. The reaction mixture was then stirred for 2 days before 2N NaOH (200 ml) was added. Aqueous layer was extracted with EtOAc (3*100 ml). The combined organic layer was dried over MgSO4 and concentration of solution provided 20.0 g of crude product (98%), with was pure enough for the further reactions., 109-07-9

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

Reference:
Patent; Bristol-Myers Squibb Company; US6469006; (2002); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 109-07-9

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

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.

Preparation of Benzoylpiperazine XXX To a stirred solution of 2-methylpiperazine (10.0 g, 0.1 mol) in dry CH2Cl2 (500 ml) under argon was added a solution of 1.0 M Me2AlCl or Et2AlCl in hexanes (100 ml, 0.1 mmol) and methyl benzoate (12.4 ml, 0.1 mmol) at room temperature. The reaction mixture was then stirred for 2 days before 2N NaOH (200 ml) was added. Aqueous layer was extracted with EtOAc (3*100 ml). The combined organic layer was dried over MgSO4 and concentration of solution provided 20.0 g of crude product (98%), with was pure enough for the further reactions., 109-07-9

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

Reference:
Patent; Bristol-Myers Squibb Company; US6469006; (2002); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 109-07-9

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

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.

Preparation of Benzoylpiperazine XXX To a stirred solution of 2-methylpiperazine (10.0 g, 0.1 mol) in dry CH2Cl2 (500 ml) under argon was added a solution of 1.0 M Me2AlCl or Et2AlCl in hexanes (100 ml, 0.1 mmol) and methyl benzoate (12.4 ml, 0.1 mmol) at room temperature. The reaction mixture was then stirred for 2 days before 2N NaOH (200 ml) was added. Aqueous layer was extracted with EtOAc (3*100 ml). The combined organic layer was dried over MgSO4 and concentration of solution provided 20.0 g of crude product (98%), with was pure enough for the further reactions., 109-07-9

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

Reference:
Patent; Bristol-Myers Squibb Company; US6469006; (2002); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 2-Methylpiperazine

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

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.

1-(t-Butoxycarbonyl)-3-methylpiperazine To a cold (-5° C.) solution of 2-methylpiperazine (5.00 g, 0.05 mole) in 200 mL of CH2 Cl2 under Ar was added a solution of di-t-butyl dicarbonate (10.9 g, 0.05 mole) in 100 mL of CH2 Cl2 over 1 h. The resulting mixture was stirred at -5° C. for 1 h and then at r.t. for 2 h. The solution was then washed (H2 O), dried (Na2 SO4) and evaporated to give an oil which was chromatographed (SiO2 /ethyl acetate then ethyl acetate-MeOH-NH4 OH 10:1:0.1) to give the product (4.30 g, 43percent) as an oil. This material was used without further purification: 1 H nmr (200 MHz, CDCl3) delta 4.15-3.75 (br s, 2H), 3.0-2.6 (m, 4H), 2.47-2.35 (m, 1H), 1.48 (s, 9H), 1.08 (d, J=6.7 Hz, 3H).

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

Reference:
Patent; Bristol-Myers Squibb Company; US5434154; (1995); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 109-07-9

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

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, 42percent). LC-MS (ESI) m/z: 201 (M+1)+., 109-07-9

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

Reference:
Patent; LEAD THERAPEUTICS, INC.; US2010/35883; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 109-07-9

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

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

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

Some tips on 2-Methylpiperazine

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

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.

3.49 g (17.0 MMOL) 4-CHLOROBENZYLBROMIDE was added dropwise to a mixture of 2.04 G (20.4 MMOL) 2-Methyl piperazine and 2.40 ml (17 MMOL) triethylamine in 60 ml DMF at room temperature. The reaction mixture was stirred for 16 hours at room temperature, the poured onto aq. sodium bicarbonate solution and extracted with ethylacetate. Purification of the crude product by flash chromatography gave 2.26 g (10.1 mmol, 59 %) of 1- (4-chloro- benzyl)-3-methyl-piperazine as colorless oil. 1H-NMR (400 MHz, DMSO-d6): 0.91 (d, 3H), 1.56 (t, 1H), 1.90 (TD, 1H), 1.91-2. 03 (m, 1 H), 2.56-2. 74, m, 4H), 2.79 (dt, 1 H), 3.40 and 3.44 (AB-Sys., 2H), 7.33 (d, 2H), 7.40 (d, 2H). MS (ESI+) : 225 [M+H] +, 109-07-9

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

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2004/37796; (2004); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 2-Methylpiperazine

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

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.

A mixture of 5-chloroindole-2-carboxylic acid (0.196 g) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.288 g) in dichloromethane (10 mL) was treated with 2-Methyl-piperazine (0.15 g) and stirred at ambient temperature for 16 h. The reaction mixture was poured into dichloromethane (50 mL), washed with water, saturated sodium hydrogencarbonate solution and then brine, dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified via silica gel chromatography (0-10% methanol/dichloromethane) to give the title compound (0.229 g). 1H NMR (400 MHz, CDCl3): delta 10.99 (br s, 1 H), 7.55 (d, J = 1.76 Hz, 1 H), 7.33 (d, J = 8.80 Hz, 1 H), 7.14 (dd, J = 1.96, 6.65 Hz, 1 H), 6.63 (br s, 1 H), 4.55 (br s, 2H), 3.23-2.61 (m, 5H), 1.76 (br s, 1 H), 1.08 (d, J = 5.87 Hz, 1 H). MS (electrospray): exact mass calculated for C14H16ClN3O, 277.10; m/z found, 278.1 [M+H]+, 109-07-9

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

Reference:
Patent; Janssen Pharmaceuticals, Inc.; CARRUTHERS, Nicholas, I.; CHAI, Wenying; DVORAK, Curt, A.; EDWARDS, James, P.; GRICE, Cheryl, A.; JABLONOWSKI, Jill, A.; KARLSSON, Lars; KHATUYA, Haripada; KREISBERG, Jennifer, D.; KWOK, Annette, K.; LOVENBERG, Timothy, W.; LY, Kiev, S.; PIO, Barbara; SHAH, Chandravadan, R.; SUN, Siquan; THURMOND, Robin, L.; WEI, Jianmei; XIAO, Wei; (87 pag.)EP1373204; (2016); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Some tips on 109-07-9

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

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 30 2-(2-Methoxyphenoxy)-1-methylethyl 3-(3-methyl-1-piperazinyl)-2-pyrazinyl Ether The title compound was prepared according to the procedure described in Example 4, Step 2, starting from 2-chloro-3-[2-(2-methoxyphenoxy)-1-methylethoxy]pyrazine* (150 mg, 0.51 mmol) and 2-methylpiperazine (260 mg, 2.6 mmol) with the exception that a final extraction step between EtOAc and 5% aqueous NaOH was carried out. This gave 118 mg (65%) of the title product. HRMS m/z calcd for C19H26N4O3 (M)+358.2005, found 358.2018. Anal. (C19H26N4O3) C, H, N. *Prepared according to the procedure described in Example 4, Step 1., 109-07-9

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

Reference:
Patent; Biovitrum AB; US6465467; (2002); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics