Ammonia → HCID 86743351, compound

Participants

Reaction Steps

A suspension of 500 mg of 1,1-diethyl-3-(2,3-dihydro-12-formyl-6-methyl-8α-ergolinyl)urea and 460 mg of hydroxylamine-O-sulfonic acid in 5 ml of water is stirred for 20 hours at room temperature. The reaction mixture is poured on ice, set to be alkaline with 25% strength ammonia solution, and extracted with dichloromethane. The organic phase is dried (Na2SO4), concentrated, the residue chromatographed on silica gel with dichloromethane/methanol=95/5 as the eluting agent, and crystallized from ethyl acetate/pentane. Yield 26% of theory.

Provenance & Evidence