反应详情

0.026 ml of pyridin-2-carboxaldehyde was added to a nitrobenzene (0.5 ml) solution of 59 mg of 3-(2-methoxyphenoxy)-5-(pyridin-3-yloxy)-benzene-1,2-diamine at 120° C., and the reaction liquid was stirred for 1 hour at the same temperature. The reaction mixture was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate to chloroform/methanol=20/1). The solvent of the resulting fraction was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=20/1) to obtain the entitled compound as a pale yellow solid.

1. customthe reaction liquid
2. customThe reaction mixture was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate to chloroform/methanol=20/1)
3. customThe solvent of the resulting fraction was evaporated away under reduced pressure
4. customthe resulting residue was purified
5. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=20/1)