HCID 13290537, compound → HCID 15589117, compound

Participants

Reaction Steps

A solution of 2.1 g of sodium nitrite in 25 ml of water was added drop-by-drop over a 5-minute period to a stirred solution of 7.4 g of 1C in 150 ml of 12% hydrochloric acid, at 0° C. The mixture then was allowed to warm to room temperature and was stirred for 24 hours. It then was diluted with 200 ml of water and extracted with ether. The ether extract was dried (MgSO4), filtered and concentrated to dryness. The residue was absorbed on silica gel and chromatographed, using as eluent a 2:15:33 v/v/v mixture of tetrahydrofuran, ethyl acetate and hexane (hereinafter, Solvent A), to give 1, as an amber syrup.

Provenance & Evidence