HRID885857

反应详情

EQUATION

反应方程式

HRID 885857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-acetyl-benzaldehyde (1 g, 6.75 mmol), N-methyl piperazine (878 mg, 8.76 mmol) and NaBH(OAc)3 (2.14 g, 10.12 mmol) in DCM (50 ml) was stirred at room temperature for 1 h and then acetic acid (526 mg, 8.76 mmol) was added. The resulting solution was stirred at room temperature overnight and then diluted with DCM and washed with 1 M Na2CO3. The organic phase was dried over Na2SO4 and evaporated in vacuo. The crude mixture was purified by column chromatography (eluent: DCM/MeOH/NH4OH 95:5:0.2) to give 1.06 g of 1-[2-(4-methyl-piperazin-1-ylmethyl)-phenyl]-ethanone.

WORKUP

后处理

  1. stirringThe resulting solution was stirred at room temperature overnight
  2. washwashed with 1 M Na2CO3
  3. dry with materialThe organic phase was dried over Na2SO4
  4. customevaporated in vacuo
  5. customThe crude mixture was purified by column chromatography (eluent: DCM/MeOH/NH4OH 95:5:0.2)