反应详情

1.12 g (0.006 mole) of O,O-diethyldithiophosphoric acid were added dropwise to a solution of 1.28 g (0.005 mole) of 4-(3-bromophenyl)-4-oxo-2-butenoic acid in 20 ml of acetone, and then the mixture was stirred overnight at room temperature. At the end of this time, the solvent was distilled off and the residue was extracted with diethyl ether. The extract was washed with water and dried over anhydrous sodium sulphate, after which the solvent was distilled off. The residue was subjected to column chromatography through silica gel, eluted with a 4:1 by volume mixture of benzene and ethyl acetate. The resulting solid was recrystallised from a mixture of benzene and hexane, to give 1.54 g (yield 69.8%) of the desired 4-(3-bromophenyl)-2-diethoxyphosphinothioylthio-4-oxobutenoic acid, melting at 107°-111° C.

1. distillationAt the end of this time, the solvent was distilled off
2. extractionthe residue was extracted with diethyl ether
3. washThe extract was washed with water
4. dry with materialdried over anhydrous sodium sulphate
5. distillationafter which the solvent was distilled off
6. washeluted with a 4:1 by volume mixture of benzene and ethyl acetate
7. customThe resulting solid was recrystallised from a mixture of benzene and hexane