Reaction #2457

Reaction equation

tert-butyl magnesium chloride

phosphorus trichloride

2-butyl magnesium chloride

→

2-butyl-tert-butylchlorophosphine

Solvents

diethyl ether

diethyl ether

Conditions

Workup

1. 1
   Temperaturemaintained at between -25° C. and -30° C. in an atmosphere of dry nitrogen
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 15 min. a 2 molar solution of 2-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 2-butyl-tert-butylchlorophosphine (47 g), b.p. 74° C. under a pressure of 15 mm of mercury.

Source