تفاعل #5567

معادلة التفاعل

3-amino-1-propanol

triethylamine

methylsulfonyl chloride

→

desired product

المردود 69.8%

3-methylsulfonylamino-1-methylsulfonyloxypropane

المردود 69.8%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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).

المصدر