Ethanol → Sodium 1,3,5-tricyclohexylbenzenesulfonate

HRID 926442

Reaktionsgleichung

[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

Reaktionsbedingungen

Temperatur: 3 °C

Versuchsvorschrift

30 g of tricyclohexylbenzene was dissolved in 50 ml of methylene chloride, followed by cooling/stirring at 3° C., and 15.2 g of chlorosulfonic acid was slowly added dropwise. After the dropwise addition, the mixture was stirred at room temperature for 5 hours, charged with 10 g of ice, and further charged with 40 g of an aqueous 50% sodium hydroxide solution. Furthermore, 20 g of ethanol was added, followed by stirring at 50° C. for 1 hour, and after removing insoluble matters by filtration, the filtrate was distilled off under reduced pressure at 40° C. The precipitated crystal was collected by filtration and subjected to hexane washing to obtain 30 g of sodium 1,3,5-tricyclohexylbenzenesulfonate.

Aufarbeitung

additionAfter the dropwise addition
stirringthe mixture was stirred at room temperature for 5 hours
stirringby stirring at 50° C. for 1 hour
customafter removing insoluble matters
filtrationby filtration
distillationthe filtrate was distilled off under reduced pressure at 40° C
filtrationThe precipitated crystal was collected by filtration

Quellen und Nachweise

ORD-Eintrag: ord-07db6bcd88354a1789b97d2ed4991738
Quelldatensatz: uspto-grants-2016_03
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09285679B2

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