Reaction #2456

Reaction equation

tert-butyl magnesium chloride

phosphorus trichloride

n-butyl magnesium chloride

→

n-butyl tert-butyl chlorophosphine

Solvents

diethyl ether

diethyl ether

Conditions

Workup

1. 1
   workup.ADDITIONwas added during 45 min
2. 2
   Otherto reach ambient temperature
3. 3
   Temperatureunder reflux for 30 min.
4. 4
   Temperaturecooled
5. 5
   Filtrationfiltered
6. 6
   Otherto remove magnesium chloride
7. 7
   workup.DISTILLATIONdistilled

Procedure

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.

Source