Ethanol → Sodium 1,3,5-tricyclohexylbenzenesulfonate

HRID 590895

반응식

HRID 590895 반응식
[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]

참가 물질

6

반응물 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 24638Chlorosulfonic acidHCID 3015433Tricyclohexylbenzene

생성물 1

HCID 86655172Sodium 1,3,5-tricyclohexylbenzenesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
3 °C

실험 절차

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 into the solution. After the completion of the dropping, the mixture was agitated at room temperature for five hours. Subsequently, 10 g of ice and then 40 g of 50% aqueous sodium hydroxide solution was poured into the mixture. Further, 20 g of ethanol was added and agitated at 50° C. for an hour. Any insoluble matter was removed by filtration, and the product was subjected to vacuum distillation at 40° C. The thus obtained crystal was collected by filtration, and washed with hexane, thereby obtaining 30 g of sodium 1,3,5-tricyclohexylbenzenesulfonate.

후처리

  1. stirringAfter the completion of the dropping, the mixture was agitated at room temperature for five hours
  2. stirringagitated at 50° C. for an hour
  3. customAny insoluble matter was removed by filtration
  4. distillationthe product was subjected to vacuum distillation at 40° C
  5. filtrationThe thus obtained crystal was collected by filtration
  6. washwashed with hexane

출처 및 근거

ORD 기록
ord-43f04fccdfa146fda9f1cee1f1fec542
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09235116B2

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