Category: 109-01-3

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.

A l-liter-3-neck flask was loaded with 4-nitrobenzoyl chloride (50.5 g, 267 mmol) and THF (500 ml) and cooled to 0 C. Pyridine (44 ml, 544 mmol), then 1-methyl-piperazine (35 ml, 316 mmol) were added while mechanically stirring at 0 C. After the addition was completed the ice bath was removed and the mixture stirred for 1 hour, while warming to room temperature. A voluminous precipitate forms. The slurry was diluted with dichloromethane and 1 M aq. KOH and the layers separated. The organic layer was washed one more time with 1 M aq. KOH, then with brine and dried over MgSO4, filtered and concentrated in vacuum. 31.5 g yellow solid (4-methylpiperazin- l-yl)(4-nitrophenyl)methanone were isolated. MS (ESI) m/z 250 (M+H). 1H NMR (CDCl3) delta ppm 8.27 (d, 2 H, J= 7.9), 7.56 (d, 2 H, /= 7.9), 3.81 (bs, 2 H), 3.37 (bs, 2 H), 2.50 (bs, 2H), 2.34 (bs, 2H), 2.32 (s, 3H)., 109-01-3

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

Reference：
Patent; BRISTOL-MYERS SQUIBB COMPANY; PURANDARE, Ashok, Vinayak; BATT, Douglas, G.; LIU, Qingjie; JOHNSON, Walter, L.; MASTALERZ, Harold; ZHANG, Guifen; ZIMMERMANN, Kurt; WO2010/80474; (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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

4-Bromobenzonitrile 52a (1.00 mmol) was placed in a reaction tube. Toluene (10 mL), Cs2CO3 (2.50 mmol), Pd2dba3 (0.03 mmol), Xphos (0.12 mmol) and piperazine (2.50 mmol) were added. The tube was sealed and the suspension was warmed to 110 C and stirred for 12 h. After this time, water was added and the mixture was extracted with EtOAc, washed with brine, dried over Na2SO4 and concentrated. The residue waxs purified by flash chromatography (hexanes/EtOAc 3:1). White solid. M.p. 186-188 C. Yield: 78%. 1H-NMR (delta, ppm): 7.44 (d, 2H, J=8.8 Hz), 6.82 (d, 2H, J=8.8 Hz), 3.31-3.29 (m, 4h), 2,53-2,51 (m, 4H), 2.31 (s, 3H).13C-NMR (delta, ppm): 153.31, 133.40, 120.04, 114.16, 100.02, 54.54, 46.99, 46.03. HRMS (ESI) [M + H]+ calculated for C12H15N3: 201.1266, found: 201.1293.

109-01-3, As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference：
Article; La Pietra, Valeria; Sartini, Stefania; Botta, Lorenzo; Antonelli, Alessandro; Ferrari, Silvia Martina; Fallahi, Poupak; Moriconi, Alessio; Coviello, Vito; Quattrini, Luca; Ke, Yi-Yu; Hsing-Pang, Hsieh; Da Settimo, Federico; Novellino, Ettore; La Motta, Concettina; Marinelli, Luciana; European Journal of Medicinal Chemistry; vol. 150; (2018); p. 491 – 505;,
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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

4-Bromobenzonitrile 52a (1.00 mmol) was placed in a reaction tube. Toluene (10 mL), Cs2CO3 (2.50 mmol), Pd2dba3 (0.03 mmol), Xphos (0.12 mmol) and piperazine (2.50 mmol) were added. The tube was sealed and the suspension was warmed to 110 C and stirred for 12 h. After this time, water was added and the mixture was extracted with EtOAc, washed with brine, dried over Na2SO4 and concentrated. The residue waxs purified by flash chromatography (hexanes/EtOAc 3:1). White solid. M.p. 186-188 C. Yield: 78%. 1H-NMR (delta, ppm): 7.44 (d, 2H, J=8.8 Hz), 6.82 (d, 2H, J=8.8 Hz), 3.31-3.29 (m, 4h), 2,53-2,51 (m, 4H), 2.31 (s, 3H).13C-NMR (delta, ppm): 153.31, 133.40, 120.04, 114.16, 100.02, 54.54, 46.99, 46.03. HRMS (ESI) [M + H]+ calculated for C12H15N3: 201.1266, found: 201.1293.

109-01-3, As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference：
Article; La Pietra, Valeria; Sartini, Stefania; Botta, Lorenzo; Antonelli, Alessandro; Ferrari, Silvia Martina; Fallahi, Poupak; Moriconi, Alessio; Coviello, Vito; Quattrini, Luca; Ke, Yi-Yu; Hsing-Pang, Hsieh; Da Settimo, Federico; Novellino, Ettore; La Motta, Concettina; Marinelli, Luciana; European Journal of Medicinal Chemistry; vol. 150; (2018); p. 491 – 505;,
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

a) Synthesis of 1-(4-methylpiperazin-1-yl)ethanone A solution of N-methylpiperazine (2.0 g, 19.97 mmol), triethylamine (3.35 mL, 23.96 mmol) and acetic anhydride (2.3 mL, 23.96 mmol) in EtOH (60 mL) was stirred at room temperature overnight. The reaction mixture was evaporated to dryness. Purification of the residue by silica gel column chromatography (CH2Cl2: MeOH mixtures of increasing polarity as eluent) afforded the desired product (2.16 g, 76%) as a yellow oil. 1H-NMR (CDCl3, 300 MHz) delta: 3.65 (t, J= 6.8 Hz, 2H), 3.49 (t, J= 6.8 Hz, 2H), 2.46-2.39 (m, 4H), 2.32 (s, 3H), 2.10 (s, 3H) ppm., 109-01-3

As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference：
Patent; Laboratorios del. Dr. Esteve, S.A.; Alcalde-Pais, Maria de las Ermitas; Almansa-Rosales, Carmen; Diaz-Fernandez, Jose-Luis; Mesquida-Estevez, Maria de les Neus; Paloma-Romeu, Laura; EP2682391; (2014); 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

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：
Patent; AstraZeneca UK Limited; US6806274; (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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.,109-01-3

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 60-70 C. under about 0.2 mm Hg to give 1-(3-hydroxypropyl)-4-methylpiperazine (17 g); NMR Spectrum: (CDCl3) 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).

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

Reference：
Patent; AstraZeneca AB; US2004/48881; (2004); A1;; ; Patent; Lambert, Christine Marie Paul; Ple, Patrick; US2004/44015; (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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.,109-01-3

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 60-70 C. under about 0.2 mm Hg to give 1-(3-hydroxypropyl)-4-methylpiperazine (17 g); NMR Spectrum: (CDCl3) 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).

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

Reference：
Patent; AstraZeneca AB; US2004/48881; (2004); A1;; ; Patent; Lambert, Christine Marie Paul; Ple, Patrick; US2004/44015; (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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

4-nitrobenzylbromide (4.30 g, 20 mmol) was dissolved in 40 ml of acetonitrile solvent,Then K2CO3 (5.52 g, 40 mmol) was added,KI (0.33 g, 2 mmol),Then, 4-methylpiperazine (2.20 g, 22 mmol) was added thereto,After 5 h, the reaction was complete.The reaction solution was concentrated and dried,And further adding 100 ml of H2O thereto,Extracted with ethyl acetate (150 ml x 3)The organic layer was collected, concentrated,4.32 g of a solid was obtained in 92% yield., 109-01-3

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

Reference：
Patent; Nantong University; Ling, Yong; Mou, Jiefei; Xu, Qibing; Feng, Jiao; Zhu, Peng; Liu, Ji; Wang, Tingting; Ge, Xiang; Liang, Shanshan; (26 pag.)CN106432235; (2017); A;,
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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

4-nitrobenzylbromide (4.30 g, 20 mmol) was dissolved in 40 ml of acetonitrile solvent,Then K2CO3 (5.52 g, 40 mmol) was added,KI (0.33 g, 2 mmol),Then, 4-methylpiperazine (2.20 g, 22 mmol) was added thereto,After 5 h, the reaction was complete.The reaction solution was concentrated and dried,And further adding 100 ml of H2O thereto,Extracted with ethyl acetate (150 ml x 3)The organic layer was collected, concentrated,4.32 g of a solid was obtained in 92% yield., 109-01-3

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

Reference：
Patent; Nantong University; Ling, Yong; Mou, Jiefei; Xu, Qibing; Feng, Jiao; Zhu, Peng; Liu, Ji; Wang, Tingting; Ge, Xiang; Liang, Shanshan; (26 pag.)CN106432235; (2017); A;,
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

A 100 mL 3-necked flask was equipped with a magnetic stirrer bar, nitrogen in- and outlet and septum. The setup was thoroughly dried using a heat gun and allowed to cool to room temperature under a nitrogen flow. Then, 4-nitrobenzoyl chloride (4.64 g, 25.0 mmol) was dissolved in dry dichloromethane (50 mL) and the solution was 10 minutes in an ice-water bath. N-methylpiperazine (2.58 g, 25.8 mmol, 1.03 eq) was added drop wise over a 10 minute time interval while stirring vigorously. The resulting suspension was stirred for 1 hour at 0 C., after which triethylamine (5.01 g, 50.0 mmol, 2.0 eq) was added and stirrring was continued at r.t. for 1 h. The reaction mixture was transferred into a separatory funnel and washed with demineralized water (3×50 mL). The organic layer was dried over Na2SO4, filtered over a paper filter and all volatiles were removed under reduced pressure using a rotary evaporator to give the desired product as a pale orange solid (5.77 g 23.1 mmol, 92%)., 109-01-3

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

Reference：
Patent; TEIJIN ARAMID B.V.; VAN DEN HEUVEL, Christiaan J.M.; VELD, Martijn Arnoldus Johannes; QUAIJTAAL, Joannes H.M.; VERHOEF, Rene P.; DE JONG, Jorrit; NIJENHUIS, Wido; (12 pag.)US2018/223077; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics