Ethanol → Sodium 1,3,5-tricyclohexylbenzenesulfonate

HRID 1530157Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1530157
[CH:1]1([C:7]2[C:8](C3CCCCC3)=[C:9]([CH:13]3[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]3)[CH:10]=[CH:11][CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[S:26]([OH:29])(=[O:28])=[O:27].[OH-].[Na+:31].[CH2:32](O)[CH3:33]>C(Cl)Cl>[CH:13]1([C:9]2([S:26]([O-:29])(=[O:28])=[O:27])[CH:8]=[C:7]([CH:1]3[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]3)[CH:12]=[C:11]([CH:33]3[CH2:32][CH2:3][CH2:2][CH2:1][CH2:6]3)[CH2:10]2)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18]1.[Na+:31]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 24638Chlorosulfonic acidHCID 3015433Tricyclohexylbenzene

Produkt 1

HCID 86655172Sodium 1,3,5-tricyclohexylbenzenesulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
3 °C

Versuchsvorschrift

Tricyclohexylbenzene (30 g) was dissolved in 50 ml of methylene chloride, and the resulting solution was cooled with stirring at 3° C. Thereto, 15.2 g of chlorosulfonic acid was gradually added dropwise. After the dropwise addition, the reaction solution was stirred at room temperature for 5 hours, and 10 g of ice was poured thereinto. Furthermore, 40 g of an aqueous 50 mass % sodium hydroxide solution was poured therein, and 20 g of ethanol was then added. This mixture was stirred at 50° C. for 1 hour, and insoluble matters were removed by filtration. The residue was distilled off under reduced pressure at 40° C., and the precipitated crystal was collected by filtration and washed with hexane to obtain 30 g of sodium 1,3,5-tricyclohexylbenzenesulfonate.

Aufarbeitung

  1. temperaturethe resulting solution was cooled
  2. additionAfter the dropwise addition
  3. stirringthe reaction solution was stirred at room temperature for 5 hours
  4. stirringThis mixture was stirred at 50° C. for 1 hour
  5. custominsoluble matters were removed by filtration
  6. distillationThe residue was distilled off under reduced pressure at 40° C.
  7. filtrationthe precipitated crystal was collected by filtration
  8. washwashed with hexane

Quellen und Nachweise

ORD-Eintrag
ord-8fcf397e0bc84d07ae738993af245900
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09090722B2

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