HRID2185686

反应详情

EQUATION

反应方程式

HRID 2185686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 3-(R/S)-methylindoline-2(R/S)-carboxylate (3.60 g, 18.8 mmol) was dissolved in butylamine (100 ml) under nitrogen and the solution was then stirred at reflux for 3 hours. After cooling the mixture, the remaining butylamine was removed under vacuum. The crude product was purified by chromatography on a column of silica gel, using a 7/3 and then a 5/5 petroleum ether/ethyl acetate mixture as eluent. Two main fractions were collected. The first was a white solid which is the trans isomer.

WORKUP

后处理

  1. temperatureat reflux for 3 hours
  2. temperatureAfter cooling the mixture
  3. customthe remaining butylamine was removed under vacuum
  4. customThe crude product was purified by chromatography on a column of silica gel
  5. customTwo main fractions were collected