HRID2052648

反应详情

EQUATION

反应方程式

HRID 2052648 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

150 g of methyl-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxylate and 750 cm3 of ethylene glycol were introduced into a balloon flask. After dissolution, 127 g of 1-ethyl-2-aminomethylpyrrolidine was added and the mixture was heated at 50° C. The resulting solution was dissolved with 2 liters of water and acidified by means of 120 cm3 of acetic acid. The precipitate formed was dried off, washed with water and then dried. The precipitate was then redissolved in 915 cm3 of hot water. The solution was filtered and then the base was precipitated with ammonia. The precipitate was dried off, washed with water and then dried. 144 g of N-(1-ethyl-2-pyrrolidyl-methyl)-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxamide was produced (M.P.: 110°-115° C.; yield: 73%).

WORKUP

后处理

  1. additionwas added
  2. customThe precipitate formed
  3. customwas dried off
  4. washwashed with water
  5. customdried
  6. dissolutionThe precipitate was then redissolved in 915 cm3 of hot water
  7. filtrationThe solution was filtered
  8. customthe base was precipitated with ammonia
  9. customThe precipitate was dried off
  10. washwashed with water
  11. customdried