HRID2417989

反应详情

EQUATION

反应方程式

HRID 2417989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-benzyloxy-4-(3-bromopropyloxy)benzene (29.4 g) and potassium phthalimide (20.4 g) in dimethylformamide (150 ml) was stirred and heated on a steam bath for 17 hours under nitrogen. The solvent was distilled in vacuo and water (250 ml) was added to the residue. The mixture was extracted with dichloromethane and the extract dried over anhydrous potassium carbonate. The solvent was evaporated in vacuo and the residue was crystallized from ethanol-acetone to give 10.9 g (31%) of 1-benzyloxy-4-(3-phthalimidopropoxy)benzene, mp 143°-145°. A second crop which was obtained by concentrating the filtrate, weighed 9.2 g (26%), mp 137°-140°. The analysis of a sample, mp 141°-143°, from an earlier run was as follows:

WORKUP

后处理

  1. temperatureheated on a steam bath for 17 hours under nitrogen
  2. distillationThe solvent was distilled in vacuo and water (250 ml)
  3. additionwas added to the residue
  4. extractionThe mixture was extracted with dichloromethane
  5. dry with materialthe extract dried over anhydrous potassium carbonate
  6. customThe solvent was evaporated in vacuo
  7. customthe residue was crystallized from ethanol-acetone