反应详情

3-{4-[2-(4-Nitro-phenyl)-ethyl]-piperazin-1-yl}-1,2-benzisothiazole (942 mg, 2.56 mmol) was dissolved in 50 mL of THF treated with triethylamine (0.3 mL) and with wet Raney nickel (0.14 g). The resulting mixture was placed on a shaker type hydrogenator, purged with hydrogen, pressurized (two re-pressurizations were needed to maintain the pressure between 3 and 17 psig) and shaken at room temperature for 64 hours. The resulting mixture was filtered to remove the catalyst then filtered a second time over celite before the filtrate was concentrated. The resultant white solid was dried in vacuo (830 mg, 2.45 mmol). Yield 96%; mp 154° C.; MS (APCI): 339 [M+H]+.

1. custompurged with hydrogen
2. temperatureto maintain the pressure between 3 and 17 psig) and
3. filtrationThe resulting mixture was filtered
4. customto remove the catalyst
5. filtrationthen filtered a second time over celite before the filtrate
6. concentrationwas concentrated
7. customThe resultant white solid was dried in vacuo (830 mg, 2.45 mmol)