Acetyl chloride → HCID 66938544, compound

Participants

Reaction Steps

Combine acetyl chloride (5 mL) and dried methanol (10 mL) at 0° C. under a nitrogen atmosphere. Stir for 1 hr. at 0° C. Add a solution of 4-(3-(2-Chloro-4-fluorobenzoylamino)phenylamino)piperidine-1-carboxylic acid t-butyl ester (Preparation 56, 72 mg, 0.161 mmol) in methanol (2 mL). Stir overnight. Concentrate under reduced pressure. Triturate with diethyl ether (1 mL) to provide a pale yellow foam of the title compound: mp 255–7° C.; mass spectrum (ion spray): m/z=348.2 (M+1). Analysis calc'd for C18H21Cl3FN3O.1.0H2O: C, 49.28; H, 5.28; N, 9.58. Found: C, 49.15; H, 4.96; N, 9.56.

Provenance & Evidence