反応 #2456

反応方程式

tert-butyl magnesium chloride

phosphorus trichloride

n-butyl magnesium chloride

→

n-butyl tert-butyl chlorophosphine

溶媒

diethyl ether

diethyl ether

反応条件

後処理

1. 1
   workup.ADDITIONwas added during 45 min
2. 2
   その他to reach ambient temperature
3. 3
   温度under reflux for 30 min.
4. 4
   温度cooled
5. 5
   ろ過filtered
6. 6
   その他to remove magnesium chloride
7. 7
   workup.DISTILLATIONdistilled

実験手順

To a solution of phosphorus 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.

出典