Perchloric Acid → HCID 12927152, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 2-bromomethylphenyl-phenylphosphonic acid (3.95 g, 0.0127 mole) and 10 ml. of 10% perchloric acid was heated at 100° C. for 4.5 hours with constant stirring. The reaction mixture was cooled to 26° C. and then extracted with methylene chloride. The methylene chloride layers were washed with brine, dried over sodium sulfate and concentrated in vacuo to yield a yellow oil. This oil was distilled in a Kugelrohr at 180° C. and 0.6 torr to yield a colorless oil. The colorless oil was slurried in anhydrous diethyl ether, cooled during which period crystallization occured and then filtered to yield 1-phenyl-1,3-dihydro-2,1-benzoxaphosphole-1-oxide (2.2 g, 76% yield) as white crystals having a melting point of 99°-101° C. and the following analysis:

Provenance & Evidence