反应详情

Ethyl 3-oxo-2-propoxyiminobutyrate (syn isomer, 15.4 g.) and sulfuryl chloride (10.6 g.) were dissolved in acetic acid (15.4 ml.), warmed at 35° to 40° C. for 10 minutes with stirring and then stirred at ambient temperature for additional 6 hours. The reaction mixture was poured into ice-water (200 ml.) and the resultant mixture was extracted twice with chloroform. The extract was washed with an aqueous solution of sodium chloride, twice a saturated aqueous solution of sodium bicarbonate and once with water in turn, dried over magnesium sulfate, and then evaporated to dryness under reduced pressure to give ethyl 4-chloro-3-oxo-2-propoxyiminobutyrate (syn isomer, 15.4 g.), oil.

1. temperaturewarmed at 35° to 40° C. for 10 minutes
2. stirringstirred at ambient temperature for additional 6 hours
3. extractionthe resultant mixture was extracted twice with chloroform
4. washThe extract was washed with an aqueous solution of sodium chloride
5. dry with materialtwice a saturated aqueous solution of sodium bicarbonate and once with water in turn, dried over magnesium sulfate
6. customevaporated to dryness under reduced pressure