反应详情

A mixture of 2-chloro-6-methylnicotinonitrile (0.215 g, 1.41 mmol) and tert-butyl N-methyl-N-(4,4,4-trifluoro-3-hydroxybutyl)carbamate (0.345 g, 1.34 mmol) in DMF (6 mL) was treated with caesium carbonate (0.875 g, 2.69 mmol) at ambient temperature. After stirring for 4 days, the mixture was diluted with water and extracted with diethyl ether. The combined organic extracts were washed (water, brine), dried, and evaporated to an orange oil/solid mixture. The crude material was purified by silica gel chromatography, eluting with 100% dichloromethane and 5% methanol/95% dichloromethane (v/v) to give the product as a yellow oil (0.156 g, 31%).

1. extractionextracted with diethyl ether
2. washThe combined organic extracts were washed (water, brine)
3. customdried
4. customevaporated to an orange oil/solid mixture
5. customThe crude material was purified by silica gel chromatography
6. washeluting with 100% dichloromethane and 5% methanol/95% dichloromethane (v/v)