Acetone → HCID 69513230, compound

Participants

Reaction Steps

The product of step 3 (476 mg 1 mmol) was dissolved in 5N hydrochloric acid (10 ml), dioxane (10 ml) and acetone (5 ml) and heated at 80° C. for 2 hours. The resulting solution was concentrated in vacuo and co-evaporated with ethanol (×3) to afford a crude solid. This was partitioned between saturated sodium bicarbonate solution and ethyl acetate. The aqueous phase was re-extracted with ethyl acetate (×2), and the combined organic extracts were washed with water (×3), brine, dried and evaporated in vacuo to a crude solid. This was purified by column chromatography (1:9:40 0.880 ammonia:thanol:dichloromethane) to afford title product (300 mg, 67%); MS (AP+) m/e 446 [M+H]+

Provenance & Evidence