反应详情

Morpholine (7.34 ml) and 3.4 -dichloro-2 -hydroxymethylpyridine (3.0 g) were heated together in a bomb at 180 ° for 4 hours. After cooling, the mixture was taken up in ethanol and evaporated under reduced pressure to remove excess amine. The residue was taken up in water and extracted with chloroform. After drying (K2CO3 ) and removal of solvent, the residue was chromatographed (silica gel, CHCl3) to give an oil which was crystallised from petroleum ether (60/80 ) to give 4 -morpholino-3 -chloro-2 -hydroxymethylpyridine, 3.24 g, m.p. 80°-2°.

1. temperatureAfter cooling
2. customevaporated under reduced pressure
3. customto remove excess amine
4. extractionextracted with chloroform
5. customAfter drying
6. custom(K2CO3 ) and removal of solvent
7. customthe residue was chromatographed (silica gel, CHCl3)
8. customto give an oil which
9. customwas crystallised from petroleum ether (60/80 )