| 摘要 |
Biphenyldicarboxylate drug intermediates 3 - methoxy - 4, 5 methyl 2 oxo benzoic acid methyl ester synthesis method , comprising the following steps: equipped with a stirrer, thermometer and reflux condenser, the reaction vessel was added 0.13mol 3-methoxy-4,5-dihydroxybenzoic acid methyl ester(2), 300ml nitromethane solution, 0.16-0.19mol diamino methane solution (3), 500ml propionitrile solution, controlling the stirring speed 130-180rpm, the solution temperature is raised to 65-70 C, continued the reaction for 5-7 h, added 300ml sodium sulfite solution, the reaction was refluxed for 4-6h, cooled, added 200ml sodium chloride solution, the organic layer was separated, the aqueous layer was washed with ethylenediamine solution, the combined organic layer was washed with salt solution, washed with cyclohexanone solution, dehydrated with dehydrating agent, recrystallized in the p-xylene solution, got crystals of 3 - methoxy - 4, 5 - methyl 2 oxo benzoic acid methyl ester. |
