HCID 86657755, compound → HCID 46847412, compound

Participants

Reaction Conditions

Reaction Steps

Copper(I) cyanide (42.9 mg, 0.479 mmol) was added to a stirred solution of 4b (200 mg, 0.368 mmol) in DMSO (4.00 mL), and the resulting mixture was heated to 180° C. for 12 h. The reaction mixture was cooled to rt, quenched with satd. aq. NH4Cl and extracted with EtOAc. The combined organics were washed with water and brine, dried (sodium sulfate) and concentrated in vacuo. The resulting crude residue was purified by preparative reversed phase HPLC on YMC Pack Pro C18 stationary phase (CH3CN/H2O as eluent, 0.05% TFA as modifier), followed by lyophilization of the purified fractions to afford the title compound 6a. m/z (ES) 490 (MH)+.

Provenance & Evidence