HRID1660002

反应详情

EQUATION

反应方程式

HRID 1660002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

82 g of dextrorotatory 1-ethyl-2-aminomethylpyrrolidine, 600 ccm of chloroform and, gradually, at a temperature of from 5°-10° C.; 200 g of 7-methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride were introduced into a balloon flask with an agitator and a thermometer. After the addition of a liter of water chloroform was distilled and then the remaining solution was filtered. The base was precipitated by the addition of 60 cm3 of 20% ammonia. The crystals formed were dried off, washed with water and then dried. 162 g of dextrorotatory N-(1-ethyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide was produced (M.P.: 136°-137° C.; yield: 66%).

WORKUP

后处理

  1. customof from 5°-10° C.
  2. distillationwas distilled
  3. filtrationthe remaining solution was filtered
  4. customThe base was precipitated by the addition of 60 cm3 of 20% ammonia
  5. customThe crystals formed
  6. customwere dried off
  7. washwashed with water
  8. customdried