Sodium Chloride → 4-Dodecylbenzenesulfonyl chloride

HRID 597125

反応式

HRID 597125 の反応式
[CH2:1]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[Cl:19][S:20](O)(=[O:22])=[O:21].C(Cl)(Cl)Cl.[Cl-].[Na+]>C(Cl)(Cl)(Cl)Cl>[CH2:1]([C:13]1[CH:14]=[CH:15][C:16]([S:20]([Cl:19])(=[O:22])=[O:21])=[CH:17][CH:18]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 6212ChloroformHCID 24638Chlorosulfonic acidHCID 31237Dodecylbenzene

生成物 1

HCID 1042154-Dodecylbenzenesulfonyl chloride

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

To a solution of 24.6 grams (0.1 mole) of n-dodecylbenzene in 150 ml of carbon tetrachloride was added with stirring 34.8 grams (0.3 mole) of chlorosulfonic acid over a 1-hour period. The reaction was exothermic with the temperature rising to 27° C. Stirring was continued for 4 hours after which the reaction mixture was carefully poured onto 1 liter of cracked ice with vigorous stirring. Chloroform (200 ml) was added and the aqueous layer was saturated with sodium chloride. The chloroform layer was separated, washed two times with 500 ml of saturated aqueous sodium chloride solution, dried over Molecular Sieves 4A and filtered. The solvent was removed in vacuo, and the resulting residue was recrystallized from 100 ml of hexane. The dried product weighed 22.6 grams and melted at 33°-35° C.

後処理

  1. customrising to 27° C
  2. customThe chloroform layer was separated
  3. washwashed two times with 500 ml of saturated aqueous sodium chloride solution
  4. dry with materialdried over Molecular Sieves 4A
  5. filtrationfiltered
  6. customThe solvent was removed in vacuo
  7. customthe resulting residue was recrystallized from 100 ml of hexane

出典と根拠

ORDレコード
ord-c3052749a39c47e69496587ab9b560af
出典データセット
uspto-grants-1977_03
特許番号
US04013621

関連ノート

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