Hydrochloric Acid → HCID 86624193, compound

Participants

Reaction Steps

To a solution of 7-chloro-3-(2,2,2-trifluoroacetyl)-6-{4-[2-(2,2,2-trifluoroethylthio)-1,1-(ethylenedioxy)ethyl]-benzylamino}-2,3,4,5-tetrahydro-1H-benzo[d]azepine (97 mg, 0.16 mmol) in anhydrous dichloromethane (0.5 mL), add a solution of 4M hydrogen chloride in dioxane (1.2 mL) and reflux overnight. Dilute with dichloromethane and wash with saturated aqueous NaHCO3. Dry the organics extracts over MgSO4, filter and concentrate in vacuo. Purify the crude mixture by chromatography on silica gel eluting with hexane/EtOAc (4:1) to obtain 7-chloro-3-(2,2,2-trifluoroacetyl)-6-[4-(2,2,2-trifluoroethylthio-methylcarbonyl)-benzylamino]-2,3,4,5-tetrahydro-1H-benzo[d]azepine (37 mg, 41%). MS (ES+) m/z: 539 (M+H)+.

Provenance & Evidence