Acetyl chloride → HCID 18175040, compound

Participants

Reaction Steps

Acetyl chloride (0.6 ml) was added dropwise to a stirred solution of the product of Example 4 (3.1 g) in dry dimethylformamide (20 ml) containing triethylamine (3.3 ml) and the resulting suspension stirred at room temperature for 30 min. The suspension was partitioned between hydrochloric acid (2 N, 100 ml) and ethyl acetate (2×100 ml) and the combined extracts were washed with sodium carbonate (2 N, 100 ml) dried (MgSO4) and evaporated in vacuo to give an oil. The oil was purified by flash chromatography eluted with chloroform:methanol (19:1) to give the title compound as a foam (0.8 g), a sample of which (0.4 g) was crystallised from a mixture of ethyl acetate and hexane to give the title compound as a crystalline solid (0.3 g) m.p. 173°-175°.

Provenance & Evidence