반응 #5573

반응 방정식

4-hydroxypiperidine

triethylamine

methanesulfonyl chloride

→

desired product

수율 89.0%

1-methylsulfonyl-4-methylsulfonyloxypiperidine

수율 89.0%

용매

methylene chloride

반응 조건

후처리

1. 1
   온도cooling
2. 2
   workup.STIRRINGthe mixture was stirred at room temperature for 1 hour
3. 3
   세척The reaction mixture was washed in turn with an aqueous saturated sodium bicarbonate solution and saturated saline
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONAfter the solvent was distilled off

실험 절차

To a solution of 4-hydroxypiperidine (5.10 g, 50 mmoles) and triethylamine (20.9 ml, 150 mmoles) in methylene chloride (150 ml) was added methanesulfonyl chloride (8.54 ml, 110 mmoles) with stirring under ice-cooling and the mixture was stirred at room temperature for 1 hour. The reaction mixture was washed in turn with an aqueous saturated sodium bicarbonate solution and saturated saline and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was solidified with ethyl acetate-n-hexane to obtain 11.45 g of the desired product (88.3%, pale yellow solid).

출처