HRID1365909

反应详情

EQUATION

反应方程式

HRID 1365909 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A solution of N-(methoxymethyl)-N-(phenylmethyl)-N-(trimethylsilyl)methylamine (8.00 g, 33.6 mmol) in CH2Cl2 (140 ml) was added drop wise, over a 30 minutes period, to a stirred solution of 1-fluoro-4-((E)-2-nitro-vinyl)-benzene (5.12 g, 30.6 mmol) and trifluoroacetic acid (0.23 ml, 3.1 mmol) in CH2Cl2 (200 ml) at 0° C. The ice bath was removed, and the solution was stirred at 25° C. for an additional 48 h. It was then concentrated and purification by flash chromatography (SiO2, EtOAc/H 1:4) afforded 6.60 g (72%) of the title compound as a light yellow oil.

WORKUP

后处理

  1. customat 0° C
  2. customThe ice bath was removed
  3. concentrationIt was then concentrated
  4. custompurification by flash chromatography (SiO2, EtOAc/H 1:4)