Ammonia → HCID 11770670, compound

Participants

Reaction Steps

300 g (1.28 mol) of 6-chloro-(6H)-dibenzo[c,e][1,2]-oxaphosphorine, dissolved in 346 ml of toluene, are added dropwise with stirring to a mixture of 76.5 g (1.663 mol) of absolute ethanol and 807 ml of toluene at -15° to -20° C. in the course of 1.5 hours. 23 g (1.35 mol) of ammonia are then introduced rapidly at this temperature. The mixture is further stirred and filtered off with suction and washed with toluene. The filtrate is concentrated by distillation at 12 mbar to an internal temperature of 75° C., finally at 1 mbar. 300 g of 6-ethoxy-(6H)-dibenzo[c,e][1,2]oxaphosphorine as solidified melt are obtained.

Provenance & Evidence