反应详情

A suspension of 1.62 g (6.5 mmol) 4-hydroxy-[2,2′]bipyrimidinyl-5-carboxylic acid ethyl ester in 16 ml POCl3 was heated at reflux for lh. The solution was cooled to RT and poured into 100 ml ice-water. The pH of the solution was adjusted to 8 with sat. NaHCO3-solution. The water phase was extracted three times with 80 ml CH2Cl2. The combined organic phases were dried (Na2SO4), filtered and evaporated. The residue was purified by chromatography (SiO2, CH2Cl2/MeOH 95:5) to give 1.43 g (82%) 4-chloro-[2,2′]bipyrimidinyl-5-carboxylic acid ethyl ester as a light brown solid, MS (EI): 264.1 (M+).

1. temperaturewas heated
2. temperatureat reflux for lh
3. extractionThe water phase was extracted three times with 80 ml CH2Cl2
4. dry with materialThe combined organic phases were dried (Na2SO4)
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by chromatography (SiO2, CH2Cl2/MeOH 95:5)