HRID5471
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
To a solution of 3-amino-1-propanol (11.47 ml, 150 mmoles) and triethylamine (46 ml, 330 mmoles) in dichloromethane (250 ml) was added methylsulfonyl chloride (25.5 ml, 330 mmoles) with stirring under ice-cooling and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed in turn with an aqueous sodium bicarbnonate and water and dried. After the solvent was distilled off, the residue was purified by column chromatography (eluent: ethyl acetate) to obtain 24.22 g of the desired product (69.8%, white crystals).
WORKUP
后处理
- temperaturecooling
- stirringthe mixture was stirred at room temperature for 30 minutes
- washThe reaction mixture was washed in turn with an aqueous sodium bicarbnonate and water
- customdried
- distillationAfter the solvent was distilled off
- customthe residue was purified by column chromatography (eluent: ethyl acetate)