反应详情

温度

80 °C

Sodium hydride (1.2 g; 60% dispersion in oil) was added portionwise to a stirred solution of 2-(2-pyrimidinyl amino)ethanol (4 g) in DMF (140 ml) under an atmosphere of nitrogen. After the vigorous reaction had subsided 4-fluorobenzaldehyde (5.35 g) was added and the solution heated to 80° C. for 20 hours. After cooling the mixture was added to water (500 ml) and extracted with diethyl ether (3×300 ml). The organic extracts were washed with brine (2×200 ml), dried (MgSO4), filtered and evaporated to dryness. Chromatography of the residue on silica gel in 2% methanol in dichloromethane afforded the title compound, which was used in the next stage without further purification.

1. customAfter the vigorous reaction
2. additionwas added
3. temperatureAfter cooling the mixture
4. extractionextracted with diethyl ether (3×300 ml)
5. washThe organic extracts were washed with brine (2×200 ml)
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customevaporated to dryness