反应详情

To a stirred and cooled (ice-bath) solution of ethyl-2-butyryl-3-(3-hydroxymethylphenylamino)acrylate (29.13 g, 0.1 mol) in pyridine was added dropwise benzoyl chloride (21.09 g, 0.15 mol). The ice bath was removed and the mixture stood for 16 hours, then evaporated, treated with chloroform (200 ml) and washed with saturated aqueous sodium bicarbonate (200 ml), water (200 ml), and 2N hydrochloric acid (2×150 ml). After drying (Na2SO4) and stirring with charcoal, the solution was filtered and evaporated to an oil, which crystallised slowly under petroleum ether (b.p. 40-60) to give the title compound (34.5 g) m.p. 59°-63°.

1. customThe ice bath was removed
2. customevaporated
3. additiontreated with chloroform (200 ml)
4. washwashed with saturated aqueous sodium bicarbonate (200 ml), water (200 ml), and 2N hydrochloric acid (2×150 ml)
5. dry with materialAfter drying (Na2SO4)
6. stirringstirring with charcoal
7. filtrationthe solution was filtered
8. customevaporated to an oil, which
9. customcrystallised slowly under petroleum ether (b.p. 40-60)