反应详情

A mixture of 4-(5-bromo-3-methylpyrid-2-yl)butylamine (11.79 g) and 2-chloro-3-nitro-5-(pyrid-3-ylmethyl)-pyridine hydrochloride (4.57 g) was refluxed in ethanol (100 ml) for 8 hours. The solvent was removed in vacuo, the residue was dissolved in water (100 ml) and then extracted with chloroform (100 ml). The chloroform extract was chromatographed on silica eluted with 5% v/v methanol in chloroform followed by recrystallisation from chloroform/hexane to give the title compound as a yellow solid, m.p. 82°-84° C.

1. customThe solvent was removed in vacuo
2. dissolutionthe residue was dissolved in water (100 ml)
3. extractionextracted with chloroform (100 ml)
4. extractionThe chloroform extract
5. customwas chromatographed on silica
6. washeluted with 5% v/v methanol in chloroform
7. customfollowed by recrystallisation from chloroform/hexane