反应 #324356

ord-ea36cede2a55439582f41fdf9e0414d9

反应方程式

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
收率 94.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solvent was evaporated
  2. 2
    workup.ADDITIONethylacetate was added
  3. 3
    过滤The precipitated DIPEA bromide was filtered off
  4. 4
    其他the filtrate was evaporated
  5. 5
    workup.ADDITIONThe residue was treated with ether

实验过程

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%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08642014B2uspto-grants-2014_02