反応 #5567

反応方程式

3-amino-1-propanol

triethylamine

methylsulfonyl chloride

→

desired product

収率 69.8%

3-methylsulfonylamino-1-methylsulfonyloxypropane

収率 69.8%

溶媒

dichloromethane

反応条件

後処理

1. 1
   温度cooling
2. 2
   workup.STIRRINGthe mixture was stirred at room temperature for 30 minutes
3. 3
   洗浄The reaction mixture was washed in turn with an aqueous sodium bicarbnonate and water
4. 4
   その他dried
5. 5
   workup.DISTILLATIONAfter the solvent was distilled off
6. 6
   その他the residue was purified by column chromatography (eluent: ethyl acetate)

実験手順

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).

出典