HRID724781

反应详情

EQUATION

反应方程式

HRID 724781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of alpha-hydroxy-gamma-butyrolactone (22.0 g) and 3-trifluoromethoxy aniline (19.0 g) was heated to 150° C. (bath temperature) for 48 hours. The mixture was allowed to cool and poured into a mixture of diethyl ether and water. After shaking, the ether layer was separated and the aqueous layer extracted with diethyl ether (x2). The combined ether extracts were washed with 2M hydrochloric acid, water and brine, then dried (MgSO4). The mixture was evaporated under reduced pressure to leave an oil, which on trituration with a mixture of diethyl ether/hexane gave the sub-title compound as an off-white solid (19.42 g).

WORKUP

后处理

  1. temperatureto cool
  2. customthe ether layer was separated
  3. extractionthe aqueous layer extracted with diethyl ether (x2)
  4. washThe combined ether extracts were washed with 2M hydrochloric acid, water and brine
  5. dry with materialdried (MgSO4)
  6. customThe mixture was evaporated under reduced pressure
  7. customto leave an oil, which on trituration