Nitric Acid → 5-Cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-4-nitro-pyrazole

HRID 622607Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 622607
[C:1]([CH2:3][C:4]([NH:6][C:7]1[N:11]([C:12]2[C:17]([Cl:18])=[CH:16][C:15]([C:19]([F:22])([F:21])[F:20])=[CH:14][C:13]=2[Cl:23])[N:10]=[CH:9][CH:8]=1)=[O:5])#[N:2].C(OC(=O)C)(=O)C.[N+:31]([O-])([OH:33])=[O:32]>C(O)(=O)C>[C:1]([CH2:3][C:4]([NH:6][C:7]1[N:11]([C:12]2[C:17]([Cl:18])=[CH:16][C:15]([C:19]([F:20])([F:22])[F:21])=[CH:14][C:13]=2[Cl:23])[N:10]=[CH:9][C:8]=1[N+:31]([O-:33])=[O:32])=[O:5])#[N:2]

Komponenten

5

Edukt 3

HCID 944Nitric AcidHCID 7918Acetic AnhydrideHCID 139850675-Cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole

Produkt 1

HCID 139850685-Cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-4-nitro-pyrazoleAusbeute 36 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

7.26 g (0.02 mol) of 5-cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole (Example 1) are taken in 70 ml of glacial acetic acid, and 2 ml of acetic anhydride and 2 ml of nitric acid are added dropwise in succession at about 10° C. A crystalline solid precipitates out of the initially clear solution after prolonged stirring. After filtration with suction, washing several times with diisopropyl ether and drying, 2.9 g (36% of theory) of 5-cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-4-nitro-pyrazole of melting point 221°-223° C. are obtained.

Aufarbeitung

  1. customA crystalline solid precipitates out of the initially clear solution
  2. filtrationAfter filtration with suction
  3. washwashing several times with diisopropyl ether
  4. customdrying

Quellen und Nachweise

ORD-Eintrag
ord-66cb4facf573415587a386fcd5e8c7cc
Quelldatensatz
uspto-grants-1988_09
Patentnummer
US04772310

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