HRID65744

反应详情

EQUATION

反应方程式

HRID 65744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-chloroethylamine hydrochloride (6.25 g) in dry dimethylformamide was added dropwise to a stirred, cooled solution of potassium tert-butoxide (8.96 g) and 5-(dimethylamino)methyl-2-furanmethanol (12.4 g) in the same solvent. After 2 hr solvent was removed, the residue basified and extracted with ethyl acetate. The residue after removal of solvent was treated in ethanol with ethanolic oxalic acid. The crystalline salt was recrystallised from ethanol to give 2-[[5-(dimethylamino)methyl-2-furanyl]methoxy]ethanamine, bis oxalate, m.p. 130°-133° (3.05 g).

WORKUP

后处理

  1. customAfter 2 hr solvent was removed
  2. extractionthe residue basified and extracted with ethyl acetate
  3. customThe residue after removal of solvent
  4. additionwas treated in ethanol with ethanolic oxalic acid
  5. customThe crystalline salt was recrystallised from ethanol