Chlorosulfonic acid → 4-Methoxy-2,3,5,6-tetramethylbenzenesulfonyl chloride

HRID 1154146

Reaktionsgleichung

Reaktionsgleichung von HRID 1154146
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([CH3:9])=[C:4]([CH3:10])[C:3]=1[O:11][CH3:12].[Cl:13][S:14](O)(=[O:16])=[O:15]>ClCCl>[CH3:12][O:11][C:3]1[C:4]([CH3:10])=[C:5]([CH3:9])[C:6]([S:14]([Cl:13])(=[O:16])=[O:15])=[C:7]([CH3:8])[C:2]=1[CH3:1]

Komponenten

4

Edukt 2

HCID 24638Chlorosulfonic acidHCID 2786643-Methoxy-1,2,4,5-tetramethylbenzene

Produkt 1

HCID 159175204-Methoxy-2,3,5,6-tetramethylbenzenesulfonyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

In 600 ml of dichloromethane was dissolved 10.0 g of 2,3,5,6-tetramethylanisole, followed by addition of a solution (400 ml) of 12 ml of chlorosulfonic acid in dichloromethane at -5°~-10° C. The mixture was kept stirred for 2 hours and the reaction mixture was poured into ice-5% aqueous NaHCO3. The organic layer was washed with water and dried over magnesium sulfate. The solvent was distilled off and the residue was crystallized from n-hexane and filtered.

Aufarbeitung

  1. washThe organic layer was washed with water
  2. dry with materialdried over magnesium sulfate
  3. distillationThe solvent was distilled off
  4. customthe residue was crystallized from n-hexane
  5. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-c254c37c89bf40f29c916ef78cc2ef2d
Quelldatensatz
uspto-grants-1984_12
Patentnummer
US04487726

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