反应详情

2.0 g (5.4 mmol) of N-[3-carboxy-phenyl]-4-(2-(3-hydroxy-propyl-amino)-4-pyridyl)-2-pyrimidineamine and 0.28 ml (5.4 mmol) of conc. sulfuric acid are boiled under RF in 150 ml of methanol for 24 h. After cooling to RT, the reaction mixture is concentrated to half the volume, diluted with 100 ml of ethyl acetate and extracted twice with 50 ml of buffer (pH 7) each time. The organic phase is dried (Na2SO4) and concentrated. Crystallisation (methylene chloride/methanol) gives N-[3-methoxycarbonylphenyl]-4-[2-(3-hydroxy-propyl-amino)-4-pyridyl]-2-pyrimidineamine; m.p. 162°-163°, FAB-MS: 380 (M+ +H).

1. concentrationthe reaction mixture is concentrated to half the volume
2. additiondiluted with 100 ml of ethyl acetate
3. extractionextracted twice with 50 ml of buffer (pH 7) each time
4. dry with materialThe organic phase is dried (Na2SO4)
5. concentrationconcentrated
6. customCrystallisation (methylene chloride/methanol)