Dichloromethane → 3-Ethoxy-4-methoxybenzoyl chloride

HRID 238060Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 238060
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[O:13][CH3:14])[C:7](O)=[O:8])[CH3:2].C(Cl)[Cl:16].C(Cl)(=O)C(Cl)=O>CN(C=O)C.C1C=CC=CC=1>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[O:13][CH3:14])[C:7]([Cl:16])=[O:8])[CH3:2]

Komponenten

6

Edukt 3

HCID 6344DichloromethaneHCID 65578Oxalyl chlorideHCID 28229573-Ethoxy-4-methoxybenzoic acid

Produkt 1

HCID 450812503-Ethoxy-4-methoxybenzoyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideKatalysatorHCID 241BenzeneLösungsmittel

Versuchsvorschrift

3-ethoxy-4-methoxybenzoic acid (5 g, 25.5 mmol) was added to a solution of CH2Cl2 (40 mL) and benzene (20 mL) in a flame-dried 150 mL round bottom flask. Anhydrous DMF (9 drops) was added and the solution was cooled on ice. Oxalyl chloride (11 mL, 128 mmol) was added dropwise, and the reaction was then allowed to warm to RT. The reaction was stirred at RT for 90 minutes, then concentrated in vacuo yield an off-white solid. The solid was placed on a high-vacuum line for 2 hours, and then taken onto the next step without further characterization.

Aufarbeitung

  1. temperaturethe solution was cooled on ice
  2. concentrationconcentrated in vacuo
  3. customyield an off-white solid
  4. waitThe solid was placed on a high-vacuum line for 2 hours

Quellen und Nachweise

ORD-Eintrag
ord-1f03044187f647448e95fefc29def7e7
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08642604B2

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