Reaktion #1483144

Reaktionsgleichung

sodium hydroxide

ethanol

chlorosulfonic acid

Tricyclohexylbenzene

→

sodium 1,3,5-tricyclohexylbenzenesulfonate

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGAfter the completion of the dropping, the mixture was agitated at room temperature for 5 hours
2. 2
   workup.ADDITIONwas added
3. 3
   workup.STIRRINGThe mixture was agitated at 50° C. for 1 hour
4. 4
   Sonstigeany undissolved matter was removed by filtration
5. 5
   workup.DISTILLATIONVacuum distillation
6. 6
   Sonstigewas carried out at 40° C.
7. 7
   Sonstigeseparated crystals
8. 8
   Filtrationwere collected by filtration
9. 9
   WaschenThe crystals were washed with hexane

Vorschrift

Tricyclohexylbenzene amounting to 30 g was dissolved in 50 ml of methylene chloride, and agitated while cooling at 3° C. Then, 15.2 g of chlorosulfonic acid was slowly dropped thereinto. After the completion of the dropping, the mixture was agitated at room temperature for 5 hours, and 10 g of ice was poured thereinto. Further, 40 g of a 50% aqueous solution of sodium hydroxide was poured into the mixture, and 20 g of ethanol was added thereto. The mixture was agitated at 50° C. for 1 hour, and any undissolved matter was removed by filtration. Vacuum distillation was carried out at 40° C., and separated crystals were collected by filtration. The crystals were washed with hexane. Thus, 30 g of sodium 1,3,5-tricyclohexylbenzenesulfonate was obtained.

Quelle