HRID1966838
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
Sodium iodide (0.45 gm, 3 mmol) and 1,8-diazabicyclo (5.4.0)undec-7-ene (0.304 gm, 2 mmol) were added to a stirred solution of [3-(benzyloxy)cyclobutyl]methyl methanesulfonate (0.27 gm, 1 mmol) (step b) in dimethoxyethane and the reaction mixture was refluxed for about 2 hours. It was allowed to come to room temperature and then was stirred with diethyl ether and water for about 10 minutes. The ether layer was separated and aqueous layer was washed with ether. The combined organic layer was washed with brine, dried over anhydrous sodium sulphate and concentrated under reduced pressure. The crude compound was purified over silica gel.
WORKUP
后处理
- temperaturethe reaction mixture was refluxed for about 2 hours
- customto come to room temperature
- customThe ether layer was separated
- washaqueous layer was washed with ether
- washThe combined organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulphate
- concentrationconcentrated under reduced pressure
- customThe crude compound was purified over silica gel