Succinic Acid → 6-(5-Amino-[1,2,4]thiadiazol-3-ylthiomethyl)-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine Succinate

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

ORD-Eintrag

ord-b6d016e0d83e443d92b557d8353e09fd

Quelldatensatz

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07994163B2