反应详情

温度

60 °C

1.65 g (14.68 mmol) of potassium tert-butoxide were suspended in 15 ml of 1,2-dimethoxyethane. After addition of 0.97 g (5.87 mmol) of 3-(hydroxymethyl)benzenecarboxylic acid (Example 66A) and 1.14 g (2.94 mmol) of 2-amino-4-[4-(2-hydroxyethoxy)phenyl]-6-(phenylsulfanyl)pyridine-3,5-dicarbonitrile (Example 35A), 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 1 using conc. hydrochloric acid. The aqueous phase was decanted from the viscous precipitate formed. The residue was purified by preparative HPLC (Chromasil, water/acetonitrile+0.1% trifluoroacetic acid). The aqueous phase was evaporated and the residue was purified by preparative HPLC (Chromasil, water/acetonitrile+0.1% trifluoroacetic acid).

1. additionwere added
2. temperatureWith ice-cooling
3. customThe aqueous phase was decanted from the viscous precipitate
4. customformed
5. customThe residue was purified by preparative HPLC (Chromasil, water/acetonitrile+0.1% trifluoroacetic acid)
6. customThe aqueous phase was evaporated
7. customthe residue was purified by preparative HPLC (Chromasil, water/acetonitrile+0.1% trifluoroacetic acid)