反应详情

温度

25 °C

To a stirred solution of propargyl aluminum bromide, prepared from 52.9 g of 80% propargyl bromide in toluene, 6.41 g of aluminum splutters activated with 70 mg of mercuric choride and 80 ml of tetrahydrofuran, was added dropwise a solution of 42.2 g of furfural dimethyl acetal [J. Org. Chem., 40, 1478 (1975)] in 30 ml of tetrahydrofuran during a 15 minute period while maintaining a temperature of. 25° to 30° C. The mixture was stirred for 20 minutes at 25° C., then partitioned with ether and ice-water. The organic layer was separated, washed with water, then aqueous sodium bicarbonate, finally with brine and dried. After evaporation the residue was distilled, giving 39.8 g of the desired compound, bp 68°-69° C. (11 mm).

1. temperaturewhile maintaining a temperature of
2. custom25° to 30° C
3. custompartitioned with ether and ice-water
4. customThe organic layer was separated
5. washwashed with water
6. dry with materialaqueous sodium bicarbonate, finally with brine and dried
7. customAfter evaporation the residue
8. distillationwas distilled