反应详情

Phenylacetylene (IX, 4.4 g) is dissolved in THF (43 ml), cooled to -78°, and treated with lithium hexamethyldisilazide (1M in THF, 43 ml). The reaction is stirred for 30 min, then a solution of ethenylidenebisphosphonic acid tetraethyl ester (10.7 g) in THF (36 ml) is added and the reaction warmed to 22° for 1 hour. The reaction is quenched with water, extracted thrice with ethyl acetate. The organics were then washed with water, hydrochloric acid (10%), saturated sodium bicarbonate, and saline, dried with magnesium sulfate, and concentrated. The concentrate is purified by distillation, bp 0.1 195°-200°.

1. temperaturecooled to -78°
2. temperaturethe reaction warmed to 22° for 1 hour
3. customThe reaction is quenched with water
4. extractionextracted thrice with ethyl acetate
5. washThe organics were then washed with water, hydrochloric acid (10%), saturated sodium bicarbonate, and saline
6. dry with materialdried with magnesium sulfate
7. concentrationconcentrated
8. distillationThe concentrate is purified by distillation, bp 0.1 195°-200°