反应详情

温度

-25 °C

To a solution of phosphorous trichloride (55 g) in dry diethyl ether (200 cm3) stirred and maintained at between -25° C. and -30° C. in an atmosphere of dry nitrogen a 2 molar solution of tert-butyl magnesium chloride in diethyl ether (200 cm3, solution supplied by Aldrich Chemical Co.) was added during 45 min. After a further 30 min., a 2 molar solution of n-butyl magnesium chloride (200 cm3, solution supplied by Aldrich Chemical Co.) was added in the same way. The suspension was stirred at -25° C. for a further 45 min., then allowed to reach ambient temperature, and finally boiled under reflux for 30 min., cooled, filtered to remove magnesium chloride, and distilled, yielding n-butyl tert-butyl chlorophosphine (30.8 g), b.p. 76-78° C. under a pressure of 15 mm of mercury.

1. additionwas added during 45 min
2. customto reach ambient temperature
3. temperatureunder reflux for 30 min.
4. temperaturecooled
5. filtrationfiltered
6. customto remove magnesium chloride
7. distillationdistilled