HRID1728175

反应详情

EQUATION

反应方程式

HRID 1728175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Under argon protection, E/Z 6-Chloro-3-[5-chloro-2-(1-ethoxycarbonyl-1-methyl-ethoxy)-benzylidene]-2-oxo-2,3-dihydro-indole-1-carboxylic acid tert-butyl ester prepared in Example 229c (8 g, 15.4 mmol) and 1-(2,5-difluoro-phenyl)-3-trimethylsilyoxy-2-aza-1,3-butadiene (30.8 mmol) were dissolved in toluene. The solution was heated at 80° C. for 5 h. Then the solution was concentrated and the residue was purified by chromatography (CH2Cl2:CH3OH=50:1) to obtain 1.7 g crude product. The crude product (50 mg) was purified again by Prep-HPLC to obtain give title compound as a white solid (12 mg).

WORKUP

后处理

  1. concentrationThen the solution was concentrated
  2. customthe residue was purified by chromatography (CH2Cl2:CH3OH=50:1)
  3. customto obtain 1.7 g crude product
  4. customThe crude product (50 mg) was purified again by Prep-HPLC
  5. customto obtain