Dimethylformamide → 2,2-Difluoro-1,3-benzodioxole-4-carbonyl chloride

HRID 2395552Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2395552
[F:1][C:2]1([F:14])[O:6][C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([C:11](O)=[O:12])[C:4]=2[O:3]1.CN(C)C=O.S(Cl)([Cl:22])=O>ClCCCl>[F:1][C:2]1([F:14])[O:6][C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([C:11]([Cl:22])=[O:12])[C:4]=2[O:3]1

Komponenten

5

Edukt 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 27740672,2-Difluoro-1,3-dioxaindane-4-carboxylic acid

Produkt 1

HCID 27740622,2-Difluoro-1,3-benzodioxole-4-carbonyl chlorideAusbeute 106 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Versuchsvorschrift

2,2-Difluoro-1,3-benzodioxole-4-carboxylic acid (15.0 g) was dissolved in 1,2-dichloroethane and N,N-dimethylformamide and thionyl chloride (10.6 g) added. The mixture was heated under reflux for 1 hour, and the solvent evaporated in vacuo. The residue was dissolved in toluene and re-evaporated to yield 2,2-difluoro-1,3-benzodioxol-4-oyl chloride (17.35 g).

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 1 hour
  3. customthe solvent evaporated in vacuo
  4. dissolutionThe residue was dissolved in toluene
  5. customre-evaporated

Quellen und Nachweise

ORD-Eintrag
ord-6f602d286afe4f3d9c9cd1f5dfbb0e88
Quelldatensatz
uspto-grants-1996_02
Patentnummer
US05489570

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