反应 #684307

ord-c3052749a39c47e69496587ab9b560af

反应方程式

ClC(Cl)Cl
Chloroform
CCCCCCCCCCCCc1ccccc1
n-dodecylbenzene
O=S(=O)(O)Cl
chlorosulfonic acid
[Cl-].[Na+]
sodium chloride
CCCCCCCCCCCCc1ccc(S(=O)(=O)Cl)cc1
p-n-Dodecylbenzenesulfonyl Chloride

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他rising to 27° C
  2. 2
    其他The chloroform layer was separated
  3. 3
    洗涤washed two times with 500 ml of saturated aqueous sodium chloride solution
  4. 4
    干燥dried over Molecular Sieves 4A
  5. 5
    过滤filtered
  6. 6
    其他The solvent was removed in vacuo
  7. 7
    其他the resulting residue was recrystallized from 100 ml of hexane

实验过程

To a solution of 24.6 grams (0.1 mole) of n-dodecylbenzene in 150 ml of carbon tetrachloride was added with stirring 34.8 grams (0.3 mole) of chlorosulfonic acid over a 1-hour period. The reaction was exothermic with the temperature rising to 27° C. Stirring was continued for 4 hours after which the reaction mixture was carefully poured onto 1 liter of cracked ice with vigorous stirring. Chloroform (200 ml) was added and the aqueous layer was saturated with sodium chloride. The chloroform layer was separated, washed two times with 500 ml of saturated aqueous sodium chloride solution, dried over Molecular Sieves 4A and filtered. The solvent was removed in vacuo, and the resulting residue was recrystallized from 100 ml of hexane. The dried product weighed 22.6 grams and melted at 33°-35° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04013621uspto-grants-1977_03