反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated on a steam bath for 17 hours under nitrogen
- distillationThe solvent was distilled in vacuo and water (250 ml)
- additionwas added to the residue
- extractionThe mixture was extracted with dichloromethane
- dry with materialthe extract dried over anhydrous potassium carbonate
- customThe solvent was evaporated in vacuo
- customthe residue was crystallized from ethanol-acetone