تفاعل #2456

معادلة التفاعل

tert-butyl magnesium chloride

phosphorus trichloride

n-butyl magnesium chloride

→

n-butyl tert-butyl chlorophosphine

المذيبات

diethyl ether

diethyl ether

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added during 45 min
2. 2
   أخرىto reach ambient temperature
3. 3
   درجة الحرارةunder reflux for 30 min.
4. 4
   درجة الحرارةcooled
5. 5
   ترشيحfiltered
6. 6
   أخرىto remove magnesium chloride
7. 7
   workup.DISTILLATIONdistilled

الإجراء التجريبي

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.

المصدر