Trimethyl orthoformate → 1-Bromo-2-(dimethoxymethyl)-4,5-dimethoxybenzene

HRID 613030

Reaktionsgleichung

Reaktionsgleichung von HRID 613030
[Br:1][C:2]1[C:7](C=O)=[CH:6][C:5]([O:10][CH3:11])=[C:4]([O:12][CH3:13])[CH:3]=1.[CH:14]([O:19][CH3:20])([O:17][CH3:18])OC>CO>[CH3:20][O:19][CH:14]([O:17][CH3:18])[C:7]1[C:2]([Br:1])=[CH:3][C:4]([O:12][CH3:13])=[C:5]([O:10][CH3:11])[CH:6]=1

Komponenten

4

Edukt 2

HCID 9005Trimethyl orthoformateHCID 793516-Bromo-3,4-dimethoxybenzaldehyde

Produkt 1

HCID 110771461-Bromo-2-(dimethoxymethyl)-4,5-dimethoxybenzene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

6-Bromo-3,4-dimethoxybenzaldehyde (470 g) is suspended in methanol (600 ml), and thereto are added trimethyl orthoformate (1025 ml) and IRA-120 (H+ -type, 10 g), and the mixture is refluxed for one hour. The mixture is cooled to room temperature, and the insoluble materials are removed by filtration, and the filtrate is concentrated under reduced pressure. The resulting residue is dissolved in ether, washed, dried, evaporated to remove the ether, and distilled under reduced pressure to give 6-bromo-3,4-dimethoxybenzaldehyde dimethyl acetal (522 g) as a main distillate (133-138° C./1 Torr).

Aufarbeitung

  1. temperaturethe mixture is refluxed for one hour
  2. customthe insoluble materials are removed by filtration
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. dissolutionThe resulting residue is dissolved in ether
  5. washwashed
  6. customdried
  7. customevaporated
  8. customto remove the ether
  9. distillationdistilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a4faae7e17ca4d15b79f5c74c0c70843
Quelldatensatz
uspto-grants-1999_12
Patentnummer
US06005106

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