反应详情

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%).

1. temperatureTo a cooled
2. customThe solvent was removed under reduced pressure
3. additionTo the resulting residue water was added
4. extractionextracted with ethyl acetate (3×20 ml)
5. extractionThe combined organic extract
6. washwas washed with water, brine
7. dry with materialdried over magnesium sulphate
8. customThe solvent was removed
9. customthe product was purified on a column of silica gel (hexane/EtOAc, 1:1)