Hydrochloric Acid → HCID 20452668, compound

Participants

Reaction Steps

A suspension of 60 g of 6-(2-bromoethoxy)-2,3-dihydro-2,2-dimethyl-4H-1,3-benzoxazin-4-one in 110 ml of benzylamine is heated, with stirring, for 30 minutes in a bath at 80°. The reaction mixture is thereupon adjusted with conc. hydrochloric acid, using ice-cooling, to a pH value of about 3, and is allowed to stand until crystallisation occurs. The crystals are filtered off with suction after 4 hours, washed with 100 ml each of water and of ethyl acetate, and dried. The crude 5-(2-benzylamino-ethoxy)-salicylamide hydrochloride obtained melts at 214°-216°. The base liberated therefrom melts at 107°-108° (from ethyl acetate/ether).

Provenance & Evidence