Analyzing the synthesis route of 1-Methylpiperazine

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

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

The 1-(2-hydroxyethyl)-4-methylpiperazine used as a stating material was prepared as follows: [00711] A mixture of 2-bromoethanol (2.36 g), N-methylpiperzine (1.26 g), potassium carbonate (5.0 g) and ethanol (150 ml) was stirred and heated to reflux for 1.8 hours. The mixture was cooled to ambient temperature and filtered. The filtrate was evaporated and the residue was triturated under a mixture of methylene chloride and acetone. The resultant mixture was filtered and the filtrate was evaporated to give the required starting material as an oil (0.87 g); NMR Spectrum: (CDCl3) 2.18 (s, 3H), 2.3-2.7 (br m, 8H), 2.56 (t, 2H), 3.61 (t, 2H)., 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; AstraZeneca UK Limited; US6806274; (2004); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 1-Methylpiperazine

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

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

The starting material was prepared as follows: 3-Bromopropan-1-ol (20 ml, 20 mmol) was added dropwise to a solution of 1-methylpiperazine (29 ml, 26 mmol) in ethanol (200 ml). Potasium carbonate (83 gr, 60 mmol) was added and the mixture was refluxed for 20 hours. After cooling, the solid was filtered and the filtrate was evaporated. The residue was triturated with ether, filtrate and evaporated. The residue was distilled at about 60-70 C. under about 0.2 mm Hg to give 1-(3-hydroxypropyl)-4-methylpiperazine (17 g, 53%). 1H NMR Spectrum: (CDCl3) 1.72 (m, 2H); 2.3 (s, 3H); 2.2-2.8 (in, 8H); 2.6 (t, 2H); 3.8 (t, 2H); 5.3 (br s, 11H)

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; Hennequin, Laurent Francois Andre; US2003/212055; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Some tips on 109-01-3

109-01-3 1-Methylpiperazine 53167, apiperazines compound, is more and more widely used in various fields.

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

The starting material was ptepared as follows: 2-Bromoethanol (2.36 g, 19 mmol) was added dropwise to a mixture of 1-methylpiperazine (1.26 g, 13 mmol) and potassium carbonate (5.0 g, 36 mmol) in absolute ethanol (150 ml) and the mixture heated at reflux for 18 hours. The mixture was allowed to cool and the precipitates were removed by filtration and the solvent volatiles were removed by evaporation. The residue was treated with acetone/methylene chloride, the insolubles were removed by filtration and the solvent was removed from the filtrate by evaporation to give 1-(2-hydroxyethyl)-4-methylpiperazine (870 mg, 48percent) as a light brown oil. 1H NMR Spectrum: (CDCl3) 2.1 8(s, 3H); 2.3-2.7(br m, 8H); 2.56(t, 2H); 3.61 (t, 2H) MS-ESI: 145 [MH]+, 109-01-3

109-01-3 1-Methylpiperazine 53167, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Zeneca Limited; Zeneca Pharma S.A.; US6291455; (2001); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of 109-01-3

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

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

2-Chloro-N-methyl-N-(4-nitro-phenyl)-acetamide (210.0 g / 0.9185 mol) was suspended in toluene (1157.56 ml) and heated to 40C. N-Methylpiperazine (252.65 ml / 2.48 eq) was added dropwise within 30 minutes. The reaction was stirred for 2 hours at 55C. After cooling to ambient temperature, the reaction was washed with water (157.23 ml) and the organic layer diluted with iPrOH (1075.33 ml). Pd/C (18.81 g) was added and the reaction hydrogenated with ? (lbar) at 20C over night. After complete conversion the catalyst was filtered off, the filtrate concentrated to ~ 150 ml and triturated with Et20 (120.0 ml). The crystalline product was filtered off, washed with Et20 and dried under vacuum to obtain 170 g (70.5 %) of N-(4-amino-phenyl)-N-methyl-2-(4-methyl-piperazin-l-yl)-acetamide.

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; RATIOPHARM GMBH; TEVA PHARMACEUTICALS USA, INC.; ALBRECHT, Wolfgang; FISCHER, Dirk; JANSSEN, Christian; WO2012/68441; (2012); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 109-01-3

109-01-3, 109-01-3 1-Methylpiperazine 53167, 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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

The 4-CHLORO-3-CYANO-6-METHOXY-7- [3- (4-METHYLPIPERAZIN-1-YL) PROPOXY] QUINOLINE used as a starting material was prepared as follows:- A mixture of 3-bromopropanol (20 ml), N-METHYLPIPERAZINE (29 ml), potassium carbonate (83 g) and ethanol (200 ml) was stirred and heated to reflux for 20 hours. The mixture was cooled to ambient temperature and filtered. The filtrate was evaporated and the residue was triturated under diethyl ether. The resultant mixture was filtered and the filtrate was evaporated. The residue was purified by distillation at about 60-70C under about 0.2 mm Hg to give 1- (3-HYDROXYPROPYL)-4-METHYLPIPERAZINE (17 g); NMR Spectrum : (CDC13) 1.72 (m, 2H), 2.3 (s, 3H), 2.2-2. 8 (m, 8H), 2.6 (t, 2H), 3.8 (t, 2H), 5.3 (br s, 1H). A solution OF DIISOPROPYL AZODICARBOXYLATE (12.1 ml) in methylene chloride (50 ml) was added dropwise during 30 minutes to a stirred mixture OF 4-CHLORO-3-CYANO-7-HYDROXY- 6-methoxyquinoline (12 g), 1- (3-HYDROXYPROPYL)-4-METHYLPIPERAZINE (9.7 g), triphenylphosphine (16.1 g) and methylene chloride (200 ml) that had been cooled to 5C. The resultant mixture was allowed to warm to ambient temperature and was then stirred for 1 hour. Further portions of diisopropyl azodicarboxylate (1.2 ml) and triphenylphosphine (1.6 g) were added and the mixture was stirred at ambient temperature for a further 1 hour. The mixture was poured into water and the organic layer was separated, washed with a saturated brine solution, dried over magnesium sulphate and evaporated. The material so obtained was purified by column chromatography on silica using increasingly polar mixtures of methylene chloride and methanol as eluent. There was thus obtained the required starting material as a solid (14.5 g); NMR Spectrum : (DMSOd6) 1.95 (m, 2H), 2.13 (s, 3H), 2.24-2. 5 (m, 10H), 4.0 (s, 3H), 4.25 (t, 2H), 7.43 (s, 1H), 7.51 (s, 1H), 8.95 (s, 1H) ; Mass Spectrum : MASS 375 and 377.

109-01-3, 109-01-3 1-Methylpiperazine 53167, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2004/41811; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 1-Methylpiperazine

109-01-3 1-Methylpiperazine 53167, 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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

To a mixture of 4-FLUORO- benzonitrile 42B (1.0 g, 8. 25 MMOL) and K2CO3 (2.27 mg, 16.51 MMOL) in dimethyl sulfoxide (7 mL) was added 1-methyl piperazine (1.36 mL, 12. 38 MMOL) and the reaction continued as described above to afford amine 1.54 g of 45b in 93% YIELDS. 1H-NMR (500 MHz, CDC . S) : No. 2.36 (3Hs, s), 2.55 (4Hs, t, J = 4. 88 Hz), 3.35 (4Hs, t, J = 4. 88 Hz), 6. 87 (2Hs, d, J = 8. 78 Hz), 7.49 (2Hs, d, J = 8. 78 Hz); ESI-MASS : 202. 1 (M+1)., 109-01-3

109-01-3 1-Methylpiperazine 53167, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; THE UNIVERSITY OF TENNESSEE RESEARCH FOUNDATION; COLORADO STATE UNIVERSITY RESEARCH FOUNDATION; WO2005/7625; (2005); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics