반응 #5567

반응 방정식

3-amino-1-propanol

triethylamine

methylsulfonyl chloride

→

desired product

수율 69.8%

3-methylsulfonylamino-1-methylsulfonyloxypropane

수율 69.8%

용매

dichloromethane

반응 조건

후처리

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

실험 절차

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).

출처