Phosphorus oxychloride → 4-((4-Amino-6-chloropyrimidin-2-yl)amino)benzonitrile

Participants

Reaction Steps

1900 ml of phosphorus oxychloride was added to a reaction vessel, to this was added 190 g of 4-(4-amino-6-hydroxypyrimidin-2-ylamino)benzonitrile under stirring at RT. The reaction mass was slowly heated to 80-85° C. and maintained at the same temperature for 16-18 hr. After completion of the reaction, phosphorous oxychloride was distilled off and stripped with 950 ml of ethyl acetate. 1900 ml of chilled water was slowly added to the reaction mass and its pH was adjusted to 9-10 with 950 ml of 50% aqueous potassium carbonate. The solid was filtered and dried under vacuum at 55-60° C. overnight.

Provenance & Evidence