Acetyl chloride → HCID 89622258, compound

Participants

Reaction Steps

A solution of Example 63 (110 mg, 229 μmol) and acetyl chloride (32 μl, 458 μmol) in THF/dichloromethane (1:2, 3 ml) was treated with sodium carbonate (194 mg, 1.83 mmol) and stirred at rt overnight. Then, the mixture was diluted with methanol (2 ml) and water (1 ml) and stirred at rt for 1 h. After evaporation, the residue was purified by preparative RP-HPLC (Reprosil C18, gradient 10-95% acetonitrile/0.1% aq. formic acid). Lyophilization from 1,4-dioxane and re-purification by column chromatography on silica gel (dichloromethane/methanol 50:1→100% methanol) afforded 35 mg (28% of th.) of the title compound.

Provenance & Evidence