HRID1939220

反应详情

EQUATION

反应方程式

HRID 1939220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 0.409 g of 4-(4-aminobenzoyl)-5,6,7,8-tetrahydro-4H-thieno [3,2-b]azepine and 0.60 g of 2-methylphenylisocyanate in 2 ml of tetrahydrofuran is heated in an oil bath at 110° C. for 16 hours. The mixture is concentrated under vacuum and the residue chromatographed on preparative silica gel plates with ethyl acetate-hexane (1:1) as solvent to give a solid. Crystallization from ethyl acetate-hexane gives 0.33 g of white crystals, m.p. 179°-182° C.

WORKUP

后处理

  1. concentrationThe mixture is concentrated under vacuum
  2. customthe residue chromatographed on preparative silica gel plates with ethyl acetate-hexane (1:1) as solvent
  3. customto give a solid
  4. customCrystallization from ethyl acetate-hexane