반응 #81941

반응 방정식

p-toluenesulfonate

(2R,3R)-2-(2,4-difluorophenyl)-3-(4-methylenepiperidine-1-yl)-1-(1H-1,2,4-triazole-1-yl)butane-2-ol p-toluenesulfonate

sodium hydroxide

→

(2R,3R)-2-(2,4-difluorophenyl)-3-(4-methylenepiperidine-1-yl)-1-(1H-1,2,4-triazole-1-yl)butane-2-ol

수율 74.3%

용매

ethyl ether

반응 조건

후처리

1. 1
   건조dried over 5 g of anhydrous magnesium sulfate
2. 2
   기타the solvent was removed
3. 3
   workup.ADDITIONThere was added 40 ml of n-hexane to the residual liquid
4. 4
   기타the precipitated crystal was separated by filtration
5. 5
   기타dried

실험 절차

To 18.3 g of the p-toluenesulfonate obtained above there were added 40 ml of ethyl ether and 35 ml of 1N aqueous solution of sodium hydroxide. The organic phase was taken out, and dried over 5 g of anhydrous magnesium sulfate and then the solvent was removed. There was added 40 ml of n-hexane to the residual liquid, and the precipitated crystal was separated by filtration, and dried to obtain 9.43 g of the desired (2R,3R)-2-(2,4-difluorophenyl)-3-(4-methylenepiperidine-1-yl)-1-(1H-1,2,4-triazole-1-yl)butane-2-ol. 1H-NMR spectrum of this compound coincided with that of the compound in Example 1.

출처