反应详情

Add succinic acid (0.035 g, 0.299 mmol) to a mixture of 6-(5-amino-[1,2,4]thiadiazol-3-ylthiomethyl)-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine (0.098 g, 0.299 mmol) in absolute ethanol (5 mL), DCM (5 mL) and methanol (2 mL) at room temperature. Concentrate the reaction mixture in vacuo. Combine the residue with methanol (5 mL) and DCM (5 mL) and concentrate in vacuo. Combine the residue with MTBE (5 mL) and concentrate three times to afford a white solid. Dry under high vacuum at room temperature overnight to afford the title compound (0.133 g, 100%) as a white solid. MS (ES+) m/z: 327.0 (M+H)+.

1. concentrationConcentrate the reaction mixture in vacuo
2. concentrationconcentrate in vacuo
3. concentrationCombine the residue with MTBE (5 mL) and concentrate three times
4. customto afford a white solid
5. customDry under high vacuum at room temperature overnight