Triphenylphosphine → Triphenylphosphane dibromide

Participants

Reaction Steps

Employing a system similar to that used in Example I, 20.8 parts (0.055 mole) 1,2-bis(difluoramino)ethyl α,β-dibromoisobutyrate is added over a period of thirty minutes to 14.45 parts (0.055 mole) triphenylphosphine in 200 ml. of anhydrous diethyl ether to give an immediate precipitate of triphenylphosphine dibromide. Another 100 ml. of anhydrous ether is added during the course of the addition to facilitate stirring of the mixture. After 18 hours the mixture is filtered free of solids followed by removal of the ether at reduced pressure on a rotary evaporator. The residue when examined by gas chromatography is found to be 97-98 percent pure. Distillation of the residue gives 7.5 parts (63 percent) of 1,2-bis(difluoramino)ethyl methacrylate (b.p. 50° C/5.5 mm. of mercury), nD20 1.3944. Identification is based on infrared spectral data and elemental analysis. The product conforms to the known 1,2-bis(difluoramino)-ethyl methacrylate. The product gives the following analysis:

Provenance & Evidence