反应详情

Sodium ethoxide solution in ethanol (0.5 M, 18 ml) was added to a solution of ethyl-p-ethoxyphenylacetate (30 g) in dry dimethyl sulphoxide (180 ml) under argon cover. The mixture was stirred for 5 minutes and dry paraformaldehyde (5.4 g) added. After 19 h stirring, acetic acid (1.5 ml) was added, the solution quenched in ice and extracted with ether. The ether layer was washed with sodium bicarbonate solution and water, dried over anhydrous sodium sulphate, and the solvent evaporated. The resulting oil crystallized from petroleum ether (40°-60°) to yield 27.8 g product m.p. 35°-36° C.

1. stirringAfter 19 h stirring
2. customthe solution quenched in ice
3. extractionextracted with ether
4. washThe ether layer was washed with sodium bicarbonate solution and water
5. dry with materialdried over anhydrous sodium sulphate
6. customthe solvent evaporated
7. customThe resulting oil crystallized from petroleum ether (40°-60°)