反应详情

温度

45 °C

4-[2-(4-Benzo[d]isothiazol-3-yl-piperazin-1-yl)-ethyl]-phenylamine was diluted to 0.3 M with anhydrous pyridine, then delivered to an 8 mL vial via pipette (0.225 mmol). Propane-1-sulfonyl chloride was diluted to 1.0 M with anhydrous dichloromethane, and added to the amine solution at rt (0.40 mmol). The solution was stirred overnight at 45° C. To the reaction mixture was added polyamine scavenging resin (0.30 mmol). The solution was stirred overnight at 45° C., then filtered into an 8 mL vial. The filtrate was evaluated by MS and concentrated via HT-12 GeneVac. Crude was purified by HPLC (30×100 mm ODS-A C(18) 5u column). Propane-1-sulfonic acid {4-[2-(4-1,2-benzisothiazol-3-yl-piperazin-1-yl)-ethyl]-phenyl}-amide was isolated in 100% purity @ 254 nm; LCMS (APCI): 445 [M+H]+

1. stirringThe solution was stirred overnight at 45° C.
2. filtrationfiltered into an 8 mL vial
3. concentrationconcentrated via HT-12 GeneVac
4. customCrude was purified by HPLC (30×100 mm ODS-A C(18) 5u column)