Acetone → HCID 53825815, compound

Participants

Reaction Steps

Ethyl chloroformate (1.87 g) in acetone (10 ml) was added to a stirred solution of the product from Stage (iv) (3.6 g) and triethylamine (1.58 g) in acetone (40 ml) and water (5 ml) at 5°. A solution of sodium azide (1.22 g) in water (10 ml) was added and the mixture was stirred for 30 min at 5°. The mixture was diluted with water and extracted with toluene. The extracts were dried, heated on a steam bath for 1 h and evaporated. The residue was heated in benzyl alcohol (21 ml) at 100° for 18 h. The mixture was then distilled in vacuo and purified by FCC using hexane/ether (7:3) as eluent to give the title compound as a colourless oil (4 g).

Provenance & Evidence