[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:8]([N:11]([CH2:15][CH3:16])[CH:12]([CH3:14])[CH3:13])([CH3:10])[CH3:9].[CH2:17]1[S:21](=[O:23])(=[O:22])[O:20][CH2:19][CH2:18]1>C(#N)C>[S:21]([CH2:17][CH2:18][CH2:19][N:1]([CH2:14][CH2:12][CH2:13][S:21]([O-:23])(=[O:22])=[O:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)([O-:20])(=[O:23])=[O:22].[CH2:15]([NH+:11]([CH:12]([CH3:14])[CH3:13])[CH:8]([CH3:10])[CH3:9])[CH3:16].[CH2:17]([NH+:1]([CH:2]([CH3:3])[CH3:7])[CH:8]([CH3:10])[CH3:9])[CH3:18]A mixture of aniline (7 mmol), N,N-diisopropylethylamine (DIPEA, 18 mmol) and propane sultone (16 mmol) was heated in a pressure tube in 10 mL of acetonitrile at 120-130° C. for 9 h under argon atmosphere. The solvent was evaporated and ethylacetate was added. The precipitated DIPEA bromide was filtered off and the filtrate was evaporated. The residue was treated with ether to give di[ethyl(diisopropyl)ammonium] 3-(3-sulfonatopropylanilino)-1-propanesulfonate as a white or pinky-white solid. Yield: 94%.
読み込み中…