Azobisisobutyronitrile → HCID 13718277, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 2.1 parts of diketene and 0.4 parts of azobisisobutyronitrile were added dropwise over 15 minutes to 18.6 parts of diphenylphosphine which was stirred and heated at 85° C. in a nitrogen atmosphere. After the addition, the reaction mixture was heated for a further 5 minutes at 85° C., then cooled to room temperature. The excess diphenylphosphine and volatile impurities were removed by distillation on a wiped wall still at a wall temperature of 85° C. and a pressure of 0.04 mb, then the residue was distilled in the wiped wall still at 120° C. and a pressure of 0.013 mb. The product, (2-oxo-4-oxetanylmethyl)-diphenylphosphine, was obtained as a colourless oil and had an absorption at 1825 cm-1 in the infra-red spectrum, characteristic of a β-lactone.

Provenance & Evidence