Methyl Chloride → 6-Benzoyl-(6H)-dibenz[c,e][1,2]oxaphosphorin 6-oxide

Participants

Reaction Conditions

Reaction Steps

56 g (0.399 mol) of benzoyl chloride were warmed to 80° to 85° C. under a nitrogen atmosphere. 92 g (0.4 mol) of 6-methoxy-(6H)-dibenz[c,e][1,2]oxaphosphorin were added dropwise over the course of 90 minutes while stirring. The temperature was then increased in steps to 130° C. It was kept at this temperature until evolution of methyl chloride could no longer be detected. The residue was digested with 70 ml of toluene at room temperature. 116 g (90% of theory) of the abovementioned compound, which, after rapid recrystallization from ethanol, had a melting point of 134° to 135° C.

Provenance & Evidence