[OH-].[Na+].O1CCOCC1.[Cl:9][C:10]1[CH:11]=[C:12]2[C:16](=[CH:17][CH:18]=1)[N:15](S(C1C=CC=CC=1)(=O)=O)[C:14]([S:28]([N:31]1[CH2:36][CH2:35][NH:34][CH:33]([CH2:37][CH3:38])[CH2:32]1)(=[O:30])=[O:29])=[CH:13]2.[Cl-].[NH4+]>C(OCC)(=O)C.O>[Cl:9][C:10]1[CH:11]=[C:12]2[C:16](=[CH:17][CH:18]=1)[NH:15][C:14]([S:28]([N:31]1[CH2:36][CH2:35][NH:34][CH:33]([CH2:37][CH3:38])[CH2:32]1)(=[O:30])=[O:29])=[CH:13]2
A 1N aqueous solution (16 ml) of sodium hydroxide was added to a 1,4-dioxane solution (200 ml) of 1-[(5-chloro-1-phenylsulfonylindol-2-yl)sulfonyl]-3-(ethyl)piperazine (3.78 g) and the resulting mixture was stirred at 80° C. for 11.5 hours. A saturated aqueous solution of ammonium chloride was added to the reaction mixture. Distilled water and ethyl acetate were then added and the water layer was extracted three time. The organic layers were combined, dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The residue was subjected to chromatography on a silica gel column (methanol:methylene chloride=1:100), followed by crystallization from tetrahydrofuran—diethyl ether, whereby the title compound (2.54 g) was obtained as needle crystals.
読み込み中…
