Ethanol → Sodium 1,3,5-tricyclohexylbenzenesulfonate

HRID 926442

反応式

HRID 926442 の反応式
[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]

参加物

6

反応物 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 24638Chlorosulfonic acidHCID 3015433Tricyclohexylbenzene

生成物 1

HCID 86655172Sodium 1,3,5-tricyclohexylbenzenesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
3 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-07db6bcd88354a1789b97d2ed4991738
出典データセット
uspto-grants-2016_03
特許番号
US09285679B2

関連ノート

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