HRID36082

反应详情

EQUATION

反应方程式

HRID 36082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.43 g of N,N-dimethyl-3,4-dihydro-6-nitro-2,2-dimethyl-2H-1-benzopyran-4-carboxamide, 0.33 g of Lawesson's reagent, and 2 ml of benzene was heated under reflux for 30 minutes. The reaction product was purified by silica gel column chromatography (CH2Cl2) and recrystallized from a mixture of ethyl acetate and n-hexane to obtain 0.33 g of N,N-dimethyl-3,4-dihydro-6-nitro-2,2-dimethyl-2H-1-benzopyran-4-carbothioamide represented by formula shown below.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 30 minutes
  3. customThe reaction product was purified by silica gel column chromatography (CH2Cl2)
  4. customrecrystallized from a mixture of ethyl acetate and n-hexane