HCID 178462204, compound → HCID 178461855, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of {(S)-1-[2-(trans-4-cyanocyclohexylamino)-4-fluorophenylcarbamoyl]ethyl}carbamic acid tert-butyl ester (195 mg, 0.48 mmol) in AcOH (2 mL) was heated at 80° C. under a nitrogen atmosphere for 1 h, then at 90° C. for 2 h and finally at 110° C. for 16 h. The volatiles were removed under reduced pressure and the resulting residue dissolved in 6N HCl (5 mL) and heated at reflux temperature for 2 h. The volatiles were removed in vacuo and the resulting residue dissolved in an aqueous solution of NaHCO3 and extracted with EtOAc (×3). The combined organic fractions were washed with water, dried and concentrated in vacuo to afford the title compound as a brown solid (100 mg, 72%). LCMS (Method C): RT 2.01 min [M+H]+ 287.1.

Provenance & Evidence