反应 #985244

ord-943b16cb7d5b46f6a0f07b568d191b7f

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

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