反应详情

A mixture of 1-(ethyloxy)-4-[(phenylmethyl)oxy]-2,3-naphthalenedicarboxylic acid (2.55 g, 6.97 mmol) and ethyl(4-aminophenyl)acetate (2.49 g, 13.9 mmol) were heated to 120° C. in acetic acid (20 ml) for 18 hours. The reaction mixture was diluted with brine and extracted with ethyl acetate twice. Combined organics were washed with water then dried over magnesium sulphate, the solvent evaporated to give a brown oil. This was purified by chromatography on silica gel, eluting with ethyl acetate (0-30%) in hexane to give the title compound as a peach coloured solid (2.63 g, 5.17 mmol). LC/MS: Rt=3.95, [MH]+ 510.

1. extractionextracted with ethyl acetate twice
2. washCombined organics were washed with water
3. dry with materialthen dried over magnesium sulphate
4. customthe solvent evaporated
5. customto give a brown oil
6. customThis was purified by chromatography on silica gel
7. washeluting with ethyl acetate (0-30%) in hexane