Phosphoric Acid → HCID 67336464, compound

Participants

Reaction Conditions

Reaction Steps

Dissolve 7-chloro-6-(1H-imidazol-2-ylthiomethyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (41.4 g, 140.9 mmol) in absolute ethanol (500 mL) and water (52 mL). Warm to 70° C. to give a solution. Stir the solution at 65 to 70° C. and add 5M phosphoric acid (28.9 mL, 144.5 mmol). Heavy crystallization occurs. Cool to room temperature, then cool to 0 to 5° C. Filter the solid and rinse with cold ethanol. Dry the collected solid in vacuo to obtain the title compound as a white solid (53.7 g, 93%). MS (APCI+) m/z: 294.25 (M+H)+. mp (DSC)=243-245° C.

Provenance & Evidence