反应详情

温度

-30 °C

To a solution of tert-butyl 2-[(2,2-dioxido-3-phenyl-2,1,3-benzothiadiazol-1(3H)-yl)methyl]morpholine-4-carboxylate (385 mg, 0.864 mmol) in methanol (5 mL) was added slowly an ethereal solution of hydrochloric acid (1M, 10 mL). The mixture was swirled for 20 minutes. All volatiles were removed under reduced pressure. The white precipitate was redissolved in minutesimal amount of methanol (˜1 mL). Isopropyl ether was added until the solution became slightly cloudy. The mixture was cooled to −30° C. in a freezer. The white solid formed was collected by decantation, washed with hexane and dried in vacuo to give 327 mg (99%) of 1-(morpholin-2-ylmethyl)-3-phenyl-1,3-dihydro-2,1,3-benzothiadiazole 2,2-dioxide hydrochloride as a white powder. MS (ESI) m/z 345.9 ([M+H]+).

1. customAll volatiles were removed under reduced pressure
2. dissolutionThe white precipitate was redissolved in minutesimal amount of methanol (˜1 mL)
3. additionIsopropyl ether was added until the solution
4. customThe white solid formed
5. customwas collected by decantation
6. washwashed with hexane
7. customdried in vacuo