Analyzing the synthesis route of 5464-12-0

The synthetic route of 5464-12-0 has been constantly updated, and we look forward to future research findings.

5464-12-0, 1-(2-Hydroxyethyl)-4-methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5464-12-0, Sodium hydride (60percent, 0.87 g, 21.80 mmol) was added to diglyme (10 mL). A solution of 2-(4-methyl-piperazin-1-yl)-ethanol (3.14 g, 21.80 mmol) in diglyme (10 mL) was added slowly. The reaction mixture was heated at 40 00 for 1 hour, 4-chloro-pyridin-2- ylamine (1.40 g, 10.9 mmol) was added and the reaction mixture was heated at 80 0 o for 1 hour, then at 15700 for 16 hours. The reaction mixture was cooled, diluted with water (20 mL), and then THF (20 mL) and NaCI were added. The organic phase was separated and the aqueous phase was extracted with THF. The combined organic phase was dried, and then the solvent was evaporated. Diethyl ether was added to the residue. The resulting solid was filtered, washed with ether, and dried to afford white solid (1.86 g, 72percent), (M+H)=237.

The synthetic route of 5464-12-0 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; ASTEX THERAPEUTICS LIMITED; SAXTY, Gordon; MURRAY, Christopher William; BERDINI, Valerio; PAGE, Lee William; ROOMANS, Susan; TAMANINI, Emiliano; BUCK, Ildiko Maria; DAY, James Edward Harvey; CARR, Maria Grazia; LEE, Lydia Yuen Wah; WO2015/4481; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

New learning discoveries about 1-(2-Hydroxyethyl)-4-methylpiperazine

As the paragraph descriping shows that 5464-12-0 is playing an increasingly important role.

5464-12-0, 1-(2-Hydroxyethyl)-4-methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5464-12-0, 10.373 g 4-bromo-2-chlorophenol (50 mmol), 14.442 g 2-(4-methylpiperazin-l-yl)ethanol (100 mmol) and 26.229 g PPh3 (100 mmol) were dissolved in 250 mL dry toluene under N2 atmosphere, then 23.027 g DTAD (100 mmol) was added. The mixture was stirred at 50 ¡ãC until no further conversion was observed. The volatiles were evaporated under reduced pressure and the residue was purified via flash chromatography using EtOAc and MeOH as eluents. MS (M+H): 333.0

As the paragraph descriping shows that 5464-12-0 is playing an increasingly important role.

Reference£º
Patent; LES LABORATOIRES SERVIER; VERNALIS (R&D) LIMITED; BALINT, Balazs; CSEKEI, Marton; SZABO, Zoltan; SZLAVIK, Zoltan; KOTSCHY, Andras; CHANRION, Maia; GENESTE, Olivier; CHEN, I-Jen; DAVIDSON, James Edward Paul; MURRAY, James Brooke; SIPOS, Szabolcs; ONDI, Levente; PROSZENYAK, Agnes; (164 pag.)WO2016/207217; (2016); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

New learning discoveries about 5464-12-0

As the paragraph descriping shows that 5464-12-0 is playing an increasingly important role.

5464-12-0, 1-(2-Hydroxyethyl)-4-methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5464-12-0, Compound 31g S6-2d was added to the reaction flask under nitrogen protection.33g 1-hydroxyethyl-4-methylpiperazine, 60g of triphenylphosphine, inject 625mL of toluene, stir to dissolve, and then add52.7 g of di-tert-butyl azodicarboxylate,The reaction was heated to 50¡ãC and stirred for 2 hours.TLC showed that the compound S6-2d was completely reacted to produce the product S6-2e with increased polarity. After the treatment, 30percent hydrochloric acid in methanol was added and 300 mL was stirred at room temperature for two hours.Filtrate the filtrate,The cake was beaten with methyl tert-butyl ether to give a filtrate.Combine the filtrate dry powder mix,Column chromatography (dichloromethane/methanol=15/1) gave 22 g of a yellow liquid.That is, compound S6-2e with a yield of 57percent

As the paragraph descriping shows that 5464-12-0 is playing an increasingly important role.

Reference£º
Patent; Douchuang (Shanghai) Pharmaceutical Technology Co., Ltd.; Wang Lei; Wang Xiaolei; Wang Zongying; Chen Da; Cao Ruqi; (20 pag.)CN107573360; (2018); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 1-(2-Hydroxyethyl)-4-methylpiperazine

The synthetic route of 5464-12-0 has been constantly updated, and we look forward to future research findings.

5464-12-0, 1-(2-Hydroxyethyl)-4-methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

2-(4-Methylpiperazin-1-yl)ethyl 4-nitrophenyl carbonate To a stirred solution of 1-(2-hydroxyethyl)piperazine (26.0 g, 0.2 mol) in DMF (200 mL) was added formic acid (752 mL, 0.2 mol) and formaldehyde (16.2 g, 0.2 mol, 37percent solution in water) The reaction mixture was cautiously heated at 100¡ã C. for 2 hours then stirred overnight at room temperature. The solvent was removed in vacuo. This procedure was repeated 3 further times to give ~100 g of product. The crude products were combined and distilled under vacuum to give, at 74¡ã C., 2-(4-methylpiperazin-1-yl)ethanol (51 g, 44percent) as a colourless liquid. Analytical LCMS: (System C, RT=0.70 min), ES+: 145.1 [MH]+. 4-Nitrophenyl chloroformate (9.85 g, 49 mmol) was dissolved in DCM (200 mL), and cooled to 0¡ã C. 2-(4-methylpiperazin-1-yl)ethanol (7.2 g, 50 mmol) and NMM (6 mL) were added, and the reaction mixture was allowed to warm gradually to room temperature over 16 hours. The reaction mixture was washed with 1M aq Na2CO3 solution until the yellow colour extracted into the aqueous layer had disappeared. The organic phase was dried (MgSO4), filtered and concentrated in vacuo to give 2-(4-methylpiperazin-1-yl)ethyl 4-nitrophenyl carbonate (10.7 g, 71percent) as a yellow oil which solidified on standing. Analytical LCMS: purity ~80percent (System C, RT=1.70 min), ES+: 310.4 [MH]+., 5464-12-0

The synthetic route of 5464-12-0 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Biovitrum AB; US2009/281087; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of 5464-12-0

As the paragraph descriping shows that 5464-12-0 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5464-12-0,1-(2-Hydroxyethyl)-4-methylpiperazine,as a common compound, the synthetic route is as follows.,5464-12-0

To a mixture of 1-(2-hydroxyethyl)-4-methylpiperazine (1.0 g, 6.9 mmol) and tetrahydrofuran (15 ml) was added sodium hydride (60percent, 277 mg, 6.9 mmol) at 0¡ãC (external temperature), and the reaction mixture was stirred at room temperature for 30 minutes. Then, to the reaction mixture was added dropwise a mixture of tributyl-iodomethyl-tin (2.0 g, 4.6 mmol) and N,N-dimethylformamide (15 ml) at 0¡ãC (external temperature). Then, the reaction mixture was stirred at room temperature for 1. 5 hours. To the reaction mixture were added water and ethyl acetate, and the organic layer was separated. The organic layer was washed with water and an aqueous saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (heptane: ethyl acetate=10:1, NH silica gel) to obtain the title compound (1.9 g, 4.2 mmol, 92percent). 1H-NMR Spectrum (CDCl3) delta (ppm): 0.89(15H, t, J=7.6Hz), 1. 25-1. 34 (6H, m), 1.46-1. 54 (6H, m), 2.28 (3H, s), 2.46 (8H, brs), 2.56(2H, t, J=5.6Hz), 3.47(2H, t, J=5.6Hz), 3.73(2H, s).

As the paragraph descriping shows that 5464-12-0 is playing an increasingly important role.

Reference£º
Patent; Eisai R&D Management Co., Ltd.; EP1867650; (2007); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics