HRID1657385

反应详情

EQUATION

反应方程式

HRID 1657385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-sulfamoyl-4-isopropylthio-5-chloroaniline (0.02 mole) and chloroacetyl chloride (0.022 mole) in dioxane (75 ml.) is heated under reflux for 24 hours. The solution then is concentrated to dryness in vacuo, the residue dissolved in ethanol (60 ml.) and heated under reflux with potassium acetate (0.022 mole) and water (10 ml.) for 2 hours. The alcohol is removed in vacuo and the solution then acidified with hydrochloric acid. The precipitated product is recrystallized from a mixture of methanol and water to provide 3-chloromethyl-6-chloro-7-isopropylthio-1,2,4-benzothiadiazine-1,1-dioxide, m.p. 248°-250° C.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 24 hours
  3. concentrationThe solution then is concentrated to dryness in vacuo
  4. dissolutionthe residue dissolved in ethanol (60 ml.)
  5. temperatureheated
  6. customThe alcohol is removed in vacuo
  7. customThe precipitated product is recrystallized from a mixture of methanol and water