반응 #1946189

반응 방정식

cyanogen bromide

(2R,3R)-2-(2,4-difluorophenyl)-3-(piperazin-1-yl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol

triethylamine

→

title compound

수율 56.0%

(2R,3R)-3-(4-Cyanopiperazin-1-yl)-2-(2,4-diflurophenyl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol

수율 56.0%

용매

acetonitrile

acetonitrile

반응 조건

후처리

1. 1
   온도To a cooled
2. 2
   기타The solvent was removed under reduced pressure
3. 3
   workup.ADDITIONTo the resulting residue water was added
4. 4
   추출extracted with ethyl acetate (3×20 ml)
5. 5
   추출The combined organic extract
6. 6
   세척was washed with water, brine
7. 7
   건조dried over magnesium sulphate
8. 8
   기타The solvent was removed
9. 9
   기타the product was purified on a column of silica gel (hexane/EtOAc, 1:1)

실험 절차

To a cooled (0° C.) mixture of (2R,3R)-2-(2,4-difluorophenyl)-3-(piperazin-1-yl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol 2 (250 mg, 0.74 mmol) and triethylamine (0.42 ml, 3 mmol) in acetonitrile (15 ml) was added cyanogen bromide (160 mg, 1.5 mmol) in acetonitrile (0.5 ml). The reaction mixture was stirred at room temperature for 18 h. The solvent was removed under reduced pressure. To the resulting residue water was added and extracted with ethyl acetate (3×20 ml). The combined organic extract was washed with water, brine and dried over magnesium sulphate. The solvent was removed and the product was purified on a column of silica gel (hexane/EtOAc, 1:1) to give the title compound as a colorless solid (150 mg, 56%).

출처