Acetyl chloride → HCID 178474363, compound

Participants

Reaction Steps

A stirred solution of the product from Example 3 (0.87 g, 0.0028 mol) in pyridine (10 ml), was cooled under nitrogen in an ice bath and treated with acetyl chloride (0.22 ml, 0.0031 mol). The mixture was kept in the ice bath for 1 hour and at ambient temperature for 20 hours. It was then concentrated in vacuo. The residue was mixed with saturated NaHCO3 and extracted with CHcl3. The extract was concentrated in vacuo and the residue was chromatographed on silica gel with 5% MeOH-0.25% NH4OH--CHcl3. The product was crystallized from MeOH-EtOAc to give 0.343 g, mp 208°-209° C. and 0.0813 g, mp 207°-208° C. of the titled product.

Provenance & Evidence