反应详情

温度

60 °C

4.72 g (42.06 mmol) of potassium tert-butoxide were suspended in 25 ml of 1,2-dimethoxyethane. After addition of 1.73 g (10.51 mmol) of 3-(hydroxymethyl)benzenecarboxylic acid (Example 66A) and 1.72 g (5.26 mmol) of 2-amino-4-phenyl-6-(phenylsulfanyl)pyridine-3,5-dicarbonitrile (Example 36A), the mixture was stirred at 60° C. overnight. After cooling of the reaction mixture, 50 ml of water were added. With ice-cooling, the clear solution was acidified to pH 6-7 using conc. hydrochloric acid. The solution was evaporated. Purification was by column chromatography on silica gel 60 (mobile phase: cyclohexane/ethyl acetate 1/1, finally acetonitrile/water 10/1).

1. additionwere added
2. temperatureWith ice-cooling
3. customThe solution was evaporated
4. customPurification