Sodium hydride → HCID 10453132, compound

Participants

Reaction Steps

1.6 g of 50% sodium hydride in an oil was added in small portions to a mixture of 10 g of ethyl 4-methyl-5-imidazolecarboxylate and 70 ml of dimethylformamide, and the resulting mixture was stirred for 30 minutes. 4.1 g of 6-methylergolin-8β-ylmethyl tosylate was added to the mixture which was then heated on a water bath for 2 hours. The solvent was distilled off under reduced pressure, and the residue was subjected to alumina column chromatography eluting with ethyl acetate to obtain ethyl 4-methyl-1-(6-methylergolin-8β-ylmethyl)-5-imidazolecarboxylate from the first fraction. The product was recrystallized from dichloromethane-diethyl ether and was colorless prisms having a melting point of 225°-227° C. Yield, 0.7 g. This compound is hereinafter referred to as Compound 15A.

Provenance & Evidence