HCID 53768224, compound → HCID 21332197, compound

Participants

Reaction Steps

A suspension of this crude amide in 200 ml of 48% hydrobromic acid in acetic acid was stirred at room temperature for several hours until it was all dissolved. The reaction mixture was then diluted with ether and the solid precipitate that formed was collected by filtration. The solid was distributed between methylene chloride and 10% sodium bicarbonate solution and the organic layer was separated and dried over potassium carbonate. The residue obtained after removal of the solvent in vacuo was chromatographed on silica gel, using toluene/ethyl acetate as solvents, to yield a crystalline product. Recrystallization of this product from nitromethane gave 2-ethyl-N-(6-amino-1-methyl-1H-(1)benzothieno[3,2-c]-pyrazol-3-yl)propanamide, m.p. 196°-197° C.

Provenance & Evidence