반응 #324356

ord-ea36cede2a55439582f41fdf9e0414d9

반응 방정식

Nc1ccccc1
aniline
CCN(C(C)C)C(C)C
N,N-diisopropylethylamine
O=S1(=O)CCCO1
propane sultone
CC[NH+](C(C)C)C(C)C.CC[NH+](C(C)C)C(C)C.O=S(=O)([O-])CCCN(CCCS(=O)(=O)[O-])c1ccccc1
di[ethyl(diisopropyl)ammonium] 3-(3-sulfonatopropylanilino)-1-propanesulfonate
수율 94.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was evaporated
  2. 2
    workup.ADDITIONethylacetate was added
  3. 3
    여과The precipitated DIPEA bromide was filtered off
  4. 4
    기타the filtrate was evaporated
  5. 5
    workup.ADDITIONThe residue was treated with ether

실험 절차

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%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08642014B2uspto-grants-2014_02