HRID906939

反应详情

EQUATION

反应方程式

HRID 906939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-(methoxymethyl)-N-(phenylmethyl)-N-(trimethylsilyl)methylamine (48.3 g, 204 mmol) and (E)-3-(3,4-difluoro-phenyl)-acrylic acid (15 g, 81.5 mmol) in THF (200 mL) was added trifluoroacetic acid (0.312 mL, 0.0041 mol) at 0° C. The mixture was gradually warmed to room temperature and stirred overnight. It was then concentrated in vaccuo and the residue was diluted with n-heptane (500 mL) followed by vigorous stirring for 1 hour. The resulted white precipitation was collected and washed with heptane affording 26 g (100%) of the title compound as a white solid. MS m/e: 318.1 (M+H+).

WORKUP

后处理

  1. concentrationIt was then concentrated in vaccuo
  2. additionthe residue was diluted with n-heptane (500 mL)
  3. stirringby vigorous stirring for 1 hour
  4. customThe resulted white precipitation
  5. customwas collected
  6. washwashed with heptane affording 26 g (100%) of the title compound as a white solid