Pentamethylbenzene → Pentamethylbenzenesulphonyl chloride

HRID 1164283

반응식

HRID 1164283 반응식
[CH3:1][C:2]1[C:3]([CH3:11])=[C:4]([CH3:10])[C:5]([CH3:9])=[C:6]([CH3:8])[CH:7]=1.[Cl:12][S:13](O)(=[O:15])=[O:14]>ClCCl>[CH3:8][C:6]1[C:7]([S:13]([Cl:12])(=[O:15])=[O:14])=[C:2]([CH3:1])[C:3]([CH3:11])=[C:4]([CH3:10])[C:5]=1[CH3:9]

참가 물질

4

반응물 2

HCID 12784PentamethylbenzeneHCID 24638Chlorosulfonic acid

생성물 1

HCID 590180Pentamethylbenzenesulphonyl chloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

In 500 ml of dichloromethane was dissolved 17.8 g of pentamethylbenzene and the solution was cooled to -5°~-10° C. A solution of 24 ml of chlorosulfonic acid in 400 ml of dichloromethane was added dropwise, and the mixture was allowed to stand at room temperature. The reaction mixture was poured into ice-5% aqueous sodium hydrogen carbonate. The organic layer was washed with water and dried over magnesium sulfate. Removal of the solvent by distillation leaves crystals which were collected by filtration and recrystallized from n-hexane. Yield 27.7 g (93.5%), m.p. 80°-81° C.

후처리

  1. temperaturethe solution was cooled to -5°~-10° C
  2. customto stand at room temperature
  3. washThe organic layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customRemoval of the solvent
  6. distillationby distillation
  7. customleaves crystals which
  8. filtrationwere collected by filtration
  9. customrecrystallized from n-hexane

출처 및 근거

ORD 기록
ord-9efd88accc034523963633bc445a77b8
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04368150

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