Ethanol → Sodium 1,3,5-tricyclohexylbenzenesulfonate
Reaction equation
[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]Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 3 °C
Procedure
Subsequently, 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. After the dropwise addition, the mixture was stirred at room temperature for 5 hours, charged with 10 g of ice and then charged with 40 g of an aqueous 50% sodium hydroxide solution. 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 at 40° C. under reduced pressure. The precipitated crystal was collected by filtration and washed with hexane to obtain 30 g of sodium 1,3,5-tricyclohexylbenzenesulfonate.
Workup
- additionAfter the dropwise addition
- stirringthe mixture was stirred at room temperature for 5 hours
- stirringthe mixture was stirred at 50° C. for 1 hour
- customInsoluble matters were removed by filtration
- distillationthe residue was distilled at 40° C. under reduced pressure
- filtrationThe precipitated crystal was collected by filtration
- washwashed with hexane
Sources & evidence
- ORD record
- ord-fd678944a96b40a28043d0030f2dce37
- Source dataset
- uspto-grants-2015_04
- Patent number
- US08999621B2
Reaction notes
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