HRID2058039

反应详情

EQUATION

反应方程式

HRID 2058039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(p-Chlorophenyl)-2,3-dihydro-3-hydroxythiazolo[3,2-a]-benzimidazole-2-acetic acid, (5.0 g.) is suspended in a solution of 100 ml. of a 6 N NCl and 200 ml. of dioxane. The mixture is heated at reflux for 18 hours. The solution is concentrated in vacuo to 50 ml. To the concentrate is added 200 ml. of water, and sufficient 4 N NaOH solution to dissolve all the solids. The alkaline solution is made acidic with acetic acid. The solid is collected, washed well with water and air-dried. The crude material is recrystallized from dimethoxyethane. The product (2.0 g.) melts at 242°-243° C.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureat reflux for 18 hours
  3. concentrationThe solution is concentrated in vacuo to 50 ml
  4. additionTo the concentrate is added 200 ml
  5. dissolutionof water, and sufficient 4 N NaOH solution to dissolve all the solids
  6. customThe solid is collected
  7. washwashed well with water
  8. customair-dried
  9. customThe crude material is recrystallized from dimethoxyethane