반응 #985244

ord-943b16cb7d5b46f6a0f07b568d191b7f

반응 방정식

[N-]=[N+]=[N-].[Na+]
sodium azide
Cc1ccc(S(=O)(=O)Cl)cc1
p-toluenesulfonyl chloride
Cc1ccc(S(=O)(=O)N=[N+]=[N-])cc1
title compound
수율 80.3%
Cc1ccc(S(=O)(=O)N=[N+]=[N-])cc1
p-toluenesulfonylazide
수율 80.3%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added dropwise at 10-25° C.
  2. 2
    기타followed by reaction at room temperature for 2.5 hours
  3. 3
    농축The reaction solution was concentrated at room temperature under reduced pressure
  4. 4
    세척The resulting oily residue was washed with H2O several times
  5. 5
    건조dried over anhydrous MgSO4
  6. 6
    기타After removing the drying agent
  7. 7
    여과by filtration

실험 절차

After dissolving sodium azide (22.5 g, 0.35 mole) in a small amount of H2O, the resulting solution was diluted with a 90% ethanol aqueous solution (130 ml). To this, an ethanol solution dissolving p-toluenesulfonyl chloride (60 g, 0.32 mole) was added dropwise at 10-25° C., followed by reaction at room temperature for 2.5 hours. The reaction solution was concentrated at room temperature under reduced pressure. The resulting oily residue was washed with H2O several times and dried over anhydrous MgSO4. After removing the drying agent by filtration, there was obtained 50.7 g of the title compound as a colorless oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE040211E1uspto-grants-2008_04