반응 #545911

반응 방정식

piperidin-4-yl (2R)-((1R)-3,3-difluorocyclopentyl)-2-hydroxy-2-phenylethanoate

formaldehyde

sodium cyanoborohydride

→

title compound

1-methylpiperidin-4-yl (2R)-2-((1R)-3,3-difluorocyclopentyl)-2-hydroxy-2-phenylethanoate

용매

methanol

methanol

ethyl acetate

반응 조건

후처리

1. 1
   기타The reaction liquid
2. 2
   세척washed successively with a saturated sodium hydrogencarbonate solution and with saturated brine
3. 3
   건조dried over anhydrous sodium sulfate
4. 4
   workup.DISTILLATIONDistilling the solvent off under reduced pressure

실험 절차

To a solution of 17 mg of piperidin-4-yl (2R)-((1R)-3,3-difluorocyclopentyl)-2-hydroxy-2-phenylethanoate and 0.03 ml of formaldehyde (35% aqueous solution) in 1 ml of methanol, 0.3 ml of advancedly prepared 0.3 M methanol solution of sodium cyanoborohydride and zinc chloride (1:0.5) was added at room temperature, followed by 30 minutes' stirring at the same temperature. The reaction liquid was diluted with ethyl acetate, washed successively with a saturated sodium hydrogencarbonate solution and with saturated brine, and dried over anhydrous sodium sulfate. Distilling the solvent off under reduced pressure, 19 mg of the title compound was obtained.

출처