Succinic Acid → 7-Chloro-6-(4-methyl-thiazol-2-ylthiomethyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine Succinate

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Reaction Steps

To a solution of 7-chloro-6-(4-methyl-thiazol-2-ylthiomethyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (0.297 g, 0.914 mmol) in absolute ethanol (10 mL), add succinic acid (0.108 g, 0.915 mmol). After acid dissolves, concentrate the reaction mixture to an oil. Add MTBE and concentrate in vacuo several times to remove ethanol. Dry the residue in oven at 45-50° C. for 2 days to afford a cloudy white oil. Dilute product in methanol and concentrate in vacuo. Add DCM to the residue and concentrate several times to remove methanol. Dry under high vacuum to afford the title compound (0.405 g, 100%) as a hygroscopic white foam. MS (ES+) m/z: 325.1 (M+H)+.

Provenance & Evidence