HCID 69429842, compound → HCID 18448665, compound

Participants

Reaction Steps

A solution of [2-(5-{2-[1-(3-trifluoromethyl-benzenesulfonyl)-pyrrolidin-2-yl]-acetylamino}-5,6,7,8-tetrahydro-naphthalen-2-yl)-allyl]-carbamic acid tert-butyl ester (72 mg, 0.12 mmol) in saturated HCl/EtOAc (3 mL) was stirred at RT for 45 min. The solvent was removed with a rotary evaporator. The crude was diluted with saturated NaHCO3 (60 mL) and extracted with CH2Cl2 (60 mL×3). The extract phase was washed with saturated NaCl, dried over Na2SO4, filtered and concentrated. Reverse phase liquid chromatography [25–100% CH3CN (0.1% TFA)-H2O (0.1% TFA)] afforded the title compound-containing fractional collections. CH3CN was removed from the combined fractional collections with a rotary evaporator. The aqueous phase was neutralized with saturated with NaHCO3 (40 mL), extracted with CH2Cl2 (40 mL×3). The extract phase was washed with saturated with NaCl, dried over Na2SO4, filtered and concentrated. The title compound was obtained as an off-white solid. MS (ESI, pos. ion) m/z: 522 (M+1).

Provenance & Evidence