Oxalyl chloride → 2,6-Difluorobenzoyl isocyanate

HRID 67057

Reaktionsgleichung

Reaktionsgleichung von HRID 67057
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4]([NH2:6])=[O:5].C(Cl)(=O)[C:13](Cl)=[O:14]>ClC(Cl)C>[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4]([N:6]=[C:13]=[O:14])=[O:5]

Komponenten

4

Edukt 2

HCID 65578Oxalyl chlorideHCID 874392,6-Difluorobenzamide

Produkt 1

HCID 27333692,6-Difluorobenzoyl isocyanate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 63651,1-DichloroethaneLösungsmittel

Versuchsvorschrift

A solution of 1.7 g. of 2,6-difluorobenzamide in 50 cc of dichloroethane was heated to 50° C. and 4.2 g. of oxalyl chloride was added dropwise with stirring and the reaction was continued for 1 hour with stirring to obtain 2,6-difluorobenzoyl isocyanate. Then, dichloroethane and excess of oxalyl chloride were distilled off under a reduced pressure. The residue was admixed with 50 cc of dioxane and a solution of 3.3 g. of 3-ethoxycarbonyl-4-(3-chloro-5-trifluoromethyl-2-pyridyloxy) aniline in dioxane was added dropwise and the reaction was continued for 2 hours with stirring. After the reaction, the reaction mixture was poured into water and the resulting crystal was filtered and washed with water and dried to obtain 4.8 g. of the object compound having a melting point of 183°-186° C.

Aufarbeitung

  1. stirringwith stirring

Quellen und Nachweise

ORD-Eintrag
ord-1e1a3187d6ab4575bb9dc5431156d266
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04344951

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