反应详情

A mixture of the product of part (i) (0.80 g) and N,N-dimethylcarbamoyl chloride (0.50 g) in dichloromethane (10 ml) was stirred at room temperature for 2 hours. Trimethylsilyl cyanide (0.50 g) was added and stirring was continued for a further 6 days. The solution was evaporated and the residue was chromatographed on silica gel. Elution with dichloromethane/ methanol (100:1) gave a product which was rechromatographed on silica gel. Elution was commenced with ether and the polarity of the eluant was gradually increased by the addition of up to 6% (by volume) of methanol. Combination and evaporation of the initial product-containing fractions gave 2-(2,4-difluorophenyl)-3-(6-cyanopyrimidin-4-yl)-1-(1H-1,2,4-triazol-l-yl)butan-2-ol, m.p. 148°-149°.

1. stirringstirring
2. waitwas continued for a further 6 days
3. customThe solution was evaporated
4. customthe residue was chromatographed on silica gel
5. washElution with dichloromethane/ methanol (100:1)
6. customgave a product which
7. customwas rechromatographed on silica gel
8. washElution
9. temperaturethe polarity of the eluant was gradually increased by the addition of up to 6% (by volume) of methanol
10. customCombination and evaporation of the
11. additioninitial product-containing fractions