反应详情

A solution of 3.2 g (12.2 mmol) 6-chloro-N-methyl-4-o-tolyl-nicotinamide in 6.7 ml (60.3 mmol)1-methylpiperazine was stirred at 100° C. for 2.5 h. The reaction mixture was cooled to r.t., treated with 10 ml 0.1N NaOH and extracted. The aqueous phase was separated and extracted twice with THF and the organic phases were washed twice with brine. The combined organic phases were dried over Na2SO4, the solvent was removed under reduced pressure and the residue purified by chromatography over silica gel (CH2Cl2:MeOH=99:1) to yield 3.3 g (83.7%) product as a beige foam.

1. extractionextracted
2. customThe aqueous phase was separated
3. extractionextracted twice with THF
4. washthe organic phases were washed twice with brine
5. dry with materialThe combined organic phases were dried over Na2SO4
6. customthe solvent was removed under reduced pressure
7. customthe residue purified by chromatography over silica gel (CH2Cl2:MeOH=99:1)