Phosphorus oxychloride → HCID 18183181, compound

Participants

Reaction Steps

0.40 g (1.05 mmol) of the acetamido compound of step C is suspended in 20 ml of methylene chloride and mixed with 0.48 ml (5.3 mmol) of phosphorus oxychloride. Then, the mixture is heated to boiling for 3 hours. After concentration by evaporation, the residue is taken up in methylene chloride (30 ml) and washed with sodium bicarbonate solution and water, dried, filtered and concentrated by evaporation. 0.38 g of solid substance, which is purified by column chromatography, is obtained (silica gel, eluant chloroform:methanol=95:5). 0.32 g (84%) of pure title compound with a melting point of 305-310° C. (decomposition) is obtained.

Provenance & Evidence