反应详情

A three-necked reaction vessel equipped with a reflux condenser, mechanically driven stirrer, nitrogen inlet and thermometer was charged with 91 g. of bis(chloromethyl)phosphinic chloride and 150 cc. tetrahydrofuran. A 280 g. portion of a tetrahydrofuran solution containing 2.0 moles of phenylmagnesium chloride per kilogram of solution was gradually added to the reaction mixture at a rate such that the temperature of the reaction mixture did not exceed 30° C. The resultant mixture was stirred for one hour following completion of the addition, at which time an excess of water was added and the organic phase isolated. The aqueous phase was extracted once with chloroform and the chloroform layer combined with the previously isolated organic layer. The organic solvents were then evaporated under reduced pressure to yield an offwhite solid which was slurried with a small amount of diethyl ether and filtered. The isolated solid material weighed 62.0 g. and melted from 135° to 137° C. The reported melting range for the compound is 141°-142° C.

1. customA three-necked reaction vessel equipped with a reflux condenser
2. additionmechanically driven stirrer, nitrogen inlet and thermometer was charged with 91 g
3. additionwas gradually added to the reaction mixture at a rate such that the temperature of the reaction mixture
4. customdid not exceed 30° C
5. additioncompletion of the addition
6. customthe organic phase isolated
7. extractionThe aqueous phase was extracted once with chloroform
8. customThe organic solvents were then evaporated under reduced pressure
9. customto yield an offwhite solid which
10. filtrationfiltered
11. custommelted from 135° to 137° C
12. customis 141°-142° C.