反应详情

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)+.

1. concentrationAfter acid dissolves, concentrate the reaction mixture to an oil
2. concentrationAdd MTBE and concentrate in vacuo several times
3. customto remove ethanol
4. customDry the residue in oven at 45-50° C. for 2 days
5. customto afford a cloudy white oil
6. concentrationDilute product in methanol and concentrate in vacuo
7. concentrationAdd DCM to the residue and concentrate several times
8. customto remove methanol
9. customDry under high vacuum