반응 #41781

반응 방정식

dimethyl sulfate

methyl5-[3-nitro-4-(2,2,2-trifluoroacetylamino)phenoxy]-pyridine-3-carboxylate

acetonitrile

sodium hydroxide

toluene

→

methyl-4-[4-(methylamino)-3-nitrophenoxy]pyridine-3-carboxylate

반응 조건

후처리

1. 1
   기타evaporated
2. 2
   세척washed with water, brine
3. 3
   기타dried
4. 4
   기타evaporated
5. 5
   기타The crude was purified by column chromatography

실험 절차

To the solution of the methyl5-[3-nitro-4-(2,2,2-trifluoroacetylamino)phenoxy]-pyridine-3-carboxylate (1 eq) in a mixture of toluene, acetonitrile and sodium hydroxide solution (50%) was added benzyltrimethylammonium chloride (1 eq) and dimethyl sulfate (1.2 eq). The biphasic mixture was stirred overnight at room temperature and evaporated. The mixture was taken up in ethyl acetate, washed with water, brine, dried and evaporated. The crude was purified by column chromatography to afford methyl-4-[4-(methylamino)-3-nitrophenoxy]pyridine-3-carboxylate. MS: MH+=303.

출처