Sodium hydride → HCID 66547112, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 3-chloro-propane-1-sulfonic acid {1-{(S)-4-(2,3-dihydro-benzo[1,4]dioxin-2-yl)-benzyl}-piperidin-4-yl}-amide (410 mg, 0.88 mmol) in DMF (5 mL) is added NaH (60% dispersion in mineral oil, 71 mg, 1.8 mmol). The reaction is heated to 80° C. for 1 h, diluted with EtOAc, washed with water and brine, dried over Na2SO4, filtered, and concentrated. The residue is purified by reversed phase HPLC eluting with a gradient of 0-80% MeCN in water (+0.1% TFA). The desired fractions are lyophilized, partitioned between saturated aqueous NaHCO3 and EtOAc. The organic layer is dried over Na2SO4, filtered and concentrated to provide the title compound (LC/MS method 1: ES+ m/z 429.4 [M+H]+, Rt=0.63 min).

Provenance & Evidence