Pentamethylbenzene → Pentamethylbenzenesulphonyl chloride

HRID 1154143

Reaktionsgleichung

Reaktionsgleichung von HRID 1154143
[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]

Komponenten

4

Edukt 2

HCID 12784PentamethylbenzeneHCID 24638Chlorosulfonic acid

Produkt 1

HCID 590180Pentamethylbenzenesulphonyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-53365cfaef18415d8d8068a311c4c69e
Quelldatensatz
uspto-grants-1984_12
Patentnummer
US04487726

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