HRID1167109

反应详情

EQUATION

反应方程式

HRID 1167109 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.095 g (0.803 mmol) of sodium hydride (55 to 65% in oil) are added to a solution of 0.4 g (0.724 mmol) of methyl 2-methyl-2-phenyl-5-{4-[(4′-trifluoromethyl-biphenyl-2-carbonyl)-amino]-piperidin-1-yl}-pentanecarboxylate in 5 ml of dimethylformamide at ambient temperature and stirred for one hour. Then 0.05 ml (0.803 mmol) of methyl iodide are added and the mixture is stirred for 14 hours. The reaction solution is poured onto water, extracted with ethyl acetate, and the organic phase is dried over sodium sulphate. The product is purified by column chromatography on silica gel (eluant: dichloromethane/methanol=5:1).

WORKUP

后处理

  1. stirringthe mixture is stirred for 14 hours
  2. additionThe reaction solution is poured onto water
  3. extractionextracted with ethyl acetate
  4. dry with materialthe organic phase is dried over sodium sulphate
  5. customThe product is purified by column chromatography on silica gel (eluant: dichloromethane/methanol=5:1)