反应详情

A solution of 3.2 g (10 mmol) of 3-methyl-2-[2-(4-cyanophenyl)ethyl]imidazo[4,5-b]pyridine-6-carboxylate in 150 mL methanol was mixed with a solution of 1.5 g lithium hydroxide in 20 mL water and stirred for 24 hours at room temperature. Then the mixture was diluted with 50 mL of water, the alcohol was distilled off and the aqueous phase was washed with ethyl acetate. After acidification with dilute hydrochloric acid, the mixture was extracted several times with dichloromethane/methanol (9:1), the organic phase was dried with sodium sulfate and the solvent was distilled off. Yield: 2.1 g beige solid (70% of theory); Rf value: 0.38 (silica gel; ethyl acetate/ethanol/ammonia=50:45:5).

1. distillationthe alcohol was distilled off
2. washthe aqueous phase was washed with ethyl acetate
3. extractionAfter acidification with dilute hydrochloric acid, the mixture was extracted several times with dichloromethane/methanol (9:1)
4. dry with materialthe organic phase was dried with sodium sulfate
5. distillationthe solvent was distilled off