HRID1966838

反应详情

EQUATION

反应方程式

HRID 1966838 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturethe reaction mixture was refluxed for about 2 hours
  2. customto come to room temperature
  3. customThe ether layer was separated
  4. washaqueous layer was washed with ether
  5. washThe combined organic layer was washed with brine
  6. dry with materialdried over anhydrous sodium sulphate
  7. concentrationconcentrated under reduced pressure
  8. customThe crude compound was purified over silica gel