反応 #1273170

ord-9e5d705099234d509ed3486e771fbf63

反応条件

温度
3°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONAfter the dropwise addition
  2. 2
    workup.STIRRINGthe mixture was stirred for 5 hours at room temperature
  3. 3
    workup.STIRRINGstirring for 1 hour at 50° C.
  4. 4
    ろ過the undissolved portion was filtered off
  5. 5
    その他removed
  6. 6
    workup.DISTILLATIONthe mixture was distilled off at reduced pressure at 40° C
  7. 7
    ろ過The precipitated crystals were filtered off
  8. 8
    洗浄washed with hexane

実験手順

In 50 ml of methylene chloride, 30 g of tricyclohexylbenzene was dissolved, cooled by 3° C. and stirred, and 15.2 g of chlorosulfonic acid was slowly added dropwise. After the dropwise addition, the mixture was stirred for 5 hours at room temperature, and after the introduction of 10 g of ice, 40 g of 50% aqueous sodium hydroxide was introduced. After a further 20 g of ethanol was added and stirring for 1 hour at 50° C., the undissolved portion was filtered off and removed and the mixture was distilled off at reduced pressure at 40° C. The precipitated crystals were filtered off and washed with hexane, and 30 g of sodium 1,3,5-tricyclohexylbenzensulfonate was obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08673538B2uspto-grants-2014_03