HRID1531399

反应详情

EQUATION

反应方程式

HRID 1531399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension (6 ml) of 2-[N-(2,4,5-trimethoxybenzoyl)amino]-4-(ethoxycarbonyl)-1,3-thiazole (3.0 g) in dimethyl sulfoxide was dissolved with heat, and N-methyl-N-hexylamine (2.3 g) was added dropwise to the solution, refluxed for 2 hours. The reaction mixture was allowed to cool, poured into a mixture of 1 N hydrochloric acid (30 ml) and ice water (30 ml), and further, water was added thereto. Crystals so precipitated were collected by filtration, washed with water, and air-dried to thereby obtain crude crystals. The crystals were followed by recrystallization from 1,4-dioxane, 2.1 g of 2-[N-(4,5-dimethoxy-2-hydroxybenzoyl)amino]-4-(ethoxycarbonyl)-1,3-thiazole was obtained (yield: 64.6%).

WORKUP

后处理

  1. temperaturewith heat
  2. temperaturerefluxed for 2 hours
  3. temperatureto cool
  4. customCrystals so precipitated
  5. filtrationwere collected by filtration
  6. washwashed with water
  7. customair-dried
  8. customto thereby obtain crude crystals
  9. customThe crystals were followed by recrystallization from 1,4-dioxane