反応 #985244

ord-943b16cb7d5b46f6a0f07b568d191b7f

反応方程式

[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
収率 80.3%
Cc1ccc(S(=O)(=O)N=[N+]=[N-])cc1
p-toluenesulfonylazide
収率 80.3%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added dropwise at 10-25° C.
  2. 2
    その他followed by reaction at room temperature for 2.5 hours
  3. 3
    濃縮The reaction solution was concentrated at room temperature under reduced pressure
  4. 4
    洗浄The resulting oily residue was washed with H2O several times
  5. 5
    乾燥dried over anhydrous MgSO4
  6. 6
    その他After removing the drying agent
  7. 7
    ろ過by filtration

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: USRE040211E1uspto-grants-2008_04