反应详情

温度

120 °C

A mixture of 5.7 g of butyl 2-bromo-3-[4-(2,4,5-trimethyl-3,6-dimethoxyphenoxy)phenyl]propionate (prepared as described in Preparation 1), 1.2 g of thiourea and 10 ml of sulfolane was heated at 120° C. for 5 hours under an atmosphere of nitrogen, and then 20 ml of ethylene glycol monomethyl ether and 10 ml of 2N aqueous hydrochloric acid were added to the resulting mixture. The mixture was then heated at 100° C. for 5 hours, after which the reaction mixture was poured into water and then extracted with benzene. The extract was washed with water and dried over anhydrous sodium sulfate. The solvent was removed from the extract by distillation under reduced pressure, and the residue thus obtained was purified by column chromatography through silica gel, using a 9:1 by volume mixture of benzene and ethyl acetate as the eluent, to give 4.7 g of the title compound as a white glassy powder softening at 47°-50° C.

1. temperatureThe mixture was then heated at 100° C. for 5 hours
2. extractionextracted with benzene
3. washThe extract was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was removed from the
6. extractionextract by distillation under reduced pressure
7. customthe residue thus obtained
8. customwas purified by column chromatography through silica gel
9. additionby volume mixture of benzene and ethyl acetate as the eluent