Ethanol → Sodium 1,3,5-tricyclohexylbenzenesulfonate

HRID 1027349

Reaktionsgleichung

Reaktionsgleichung von HRID 1027349
[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

30 g of tricyclohexylbenzene was dissolved in 50 ml of methylene chloride, and the solution was stirred under cooling at 3° C. Thereto, 15.2 g of chlorosulfonic acid was slowly added dropwise and after the dropwise addition, the reaction solution was stirred at room temperature for 5 hours. Subsequently, 10 g of ice was charged, and 40 g of an aqueous 50% sodium hydroxide solution was charged. Furthermore, 20 g of ethanol was added, and the mixture was stirred at 50° C. for 1 hour. Insoluble matters were removed by filtration, and the residue was distilled off under reduced pressure at 40° C. The precipitated crystals were collected by filtration and then washed with hexane to obtain 30 g of sodium 1,3,5-tricyclohexylbenzenesulfonate.

Aufarbeitung

  1. additionafter the dropwise addition
  2. stirringthe reaction solution was stirred at room temperature for 5 hours
  3. stirringthe mixture was stirred at 50° C. for 1 hour
  4. customInsoluble matters were removed by filtration
  5. distillationthe residue was distilled off under reduced pressure at 40° C
  6. filtrationThe precipitated crystals were collected by filtration
  7. washwashed with hexane

Quellen und Nachweise

ORD-Eintrag
ord-1ea40928f6ff43d2adaaf72d4e29f615
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08735048B2

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