Sodium Chloride → 4-Dodecylbenzenesulfonyl chloride

HRID 597125

반응식

HRID 597125 반응식
[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]

참가 물질

6

반응물 4

HCID 5234Sodium ChlorideHCID 6212ChloroformHCID 24638Chlorosulfonic acidHCID 31237Dodecylbenzene

생성물 1

HCID 1042154-Dodecylbenzenesulfonyl chloride

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c3052749a39c47e69496587ab9b560af
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04013621

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