반응 #2122507

ord-b800b823e37644b090d24a3e166623ea

반응 방정식

[Na+].[OH-]
sodium hydroxide
c1cc(C2CCCCC2)c(C2CCCCC2)c(C2CCCCC2)c1
Tricyclohexylbenzene
O=S(=O)(O)Cl
chlorosulfonic acid
CCO
ethanol
O=S(=O)([O-])C1(C2CCCCC2)C=C(C2CCCCC2)C=C(C2CCCCC2)C1.[Na+]
sodium 1,3,5-tricyclohexylbenzene sulfonate
수율 151.4%

반응 조건

온도
3°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter the dropwise addition
  2. 2
    workup.STIRRINGthe resultant was stirred at room temperature for 5 hours
  3. 3
    workup.STIRRINGThe resultant was stirred at 50° C. for an hour
  4. 4
    기타the insoluble fraction was then removed
  5. 5
    여과by filtering
  6. 6
    기타the resultant was removed by distillation under reduced pressure at 40° C
  7. 7
    기타The precipitated crystals were collected
  8. 8
    여과through filtering
  9. 9
    세척washed with hexane

실험 절차

Tricyclohexylbenzene (30 g) was dissolved in 50 ml of methylene chloride, followed by stirring under cooling at 3° C., and 15.2 g of chlorosulfonic acid was slowly added dropwise thereto. After the dropwise addition, the resultant was stirred at room temperature for 5 hours, and 10 g of ice was added thereto. Subsequently, 40 g of 50% aqueous sodium hydroxide solution was added thereto, and 20 g of ethanol was further added thereto. The resultant was stirred at 50° C. for an hour, the insoluble fraction was then removed by filtering, and the resultant was removed by distillation under reduced pressure at 40° C. The precipitated crystals were collected through filtering and washed with hexane, thereby obtaining 30 g of sodium 1,3,5-tricyclohexylbenzene sulfonate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08574814B2uspto-grants-2013_11