Ammonia → HCID 13823196, compound

Participants

Reaction Steps

A solution of 1.8 g of 3-(1-acetyl-12-bromo-2,3α-dihydro-6-methyl-8α-ergolinyl)-1,1-diethylurea in 50 ml of 1N hydrochloric acid is stirred for 4 hours at 70°-80° C. The reaction mixture is poured on 100 ml of ice, combined with 25% strength ammonia solution until the reaction is alkaline, and extracted with dichloromethane. The combined organic phases are dried over magnesium sulfate, concentrated, and the residue chromatographed on silica gel with dichloromethane/methanol in a ratio of 97:3, thus isolating 300 mg of an oily product which, for complete purification, is crystallized from ethyl acetate/diisopropyl ether. Yield: 200 mg of 3-(12-bromo-2,3α-dihydro-6-methyl-8α-ergolinyl)-1,1-diethylurea.

Provenance & Evidence