HRID2217221
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
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
To a solution of 1-(diphenylmethyl)-3-azetidinol hydrochloride (5.0 g) in DMF (25 ml), was added sodium hydride under ice-bath cooling. After 10 minute stirring at the same temperature, the mixture was allowed to warm to 25° C. and then stirred for 15 hours. EtOAc (500 ml) and water (200 ml) were poured into the mixture. The organic layer was separated, washed with water and brine, and dried over MgSO4. The solvent was removed under reduced pressure. The residue was purified by column chromatography (silica gel; 200 ml, toluene:EtOAc=15:1-8:1) to give 1-(diphenylmethyl)-3-methoxyazetidine (3.41 g).
WORKUP
后处理
- temperaturecooling
- stirringstirred for 15 hours
- customThe organic layer was separated
- washwashed with water and brine
- dry with materialdried over MgSO4
- customThe solvent was removed under reduced pressure
- customThe residue was purified by column chromatography (silica gel; 200 ml, toluene:EtOAc=15:1-8:1)