HRID345968

反应详情

EQUATION

反应方程式

HRID 345968 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 41.2 g of 5-(3-thienyl)isoxazole and 36.0 g of dimethylformamide dimethylacetal, under nitrogen, is heated on a stream bath for 4 hours. The reaction is concentrated in vacuo to give a viscous oil which solidified. The residue is dissolved in methylene chloride and passed thru a short column of hydrous magnesium silicate. On cooling, 31.76 g of the desired product is obtained, mp 118°-119°, CI-MS:m/z 206(M30). Concentrating in vacuo the methylene chloride gives an additional 20.2 g of product. (Total recovered 51.96 g, 92%).

WORKUP

后处理

  1. temperatureunder nitrogen, is heated on a stream bath for 4 hours
  2. concentrationThe reaction is concentrated in vacuo
  3. customto give a viscous oil which
  4. temperatureOn cooling