Tert-Butyl nitrite → 4-Acetyl-3-cyano-1-(2,6-dichloro-4-trifluoromethoxyphenyl)pyrazole

HRID 377664Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 377664
[C:1]([C:4]1[C:5]([C:23]#[N:24])=[N:6][N:7]([C:10]2[C:15]([Cl:16])=[CH:14][C:13]([O:17][C:18]([F:21])([F:20])[F:19])=[CH:12][C:11]=2[Cl:22])[C:8]=1N)(=[O:3])[CH3:2].C(ON=O)(C)(C)C>O1CCCC1>[C:1]([C:4]1[C:5]([C:23]#[N:24])=[N:6][N:7]([C:10]2[C:15]([Cl:16])=[CH:14][C:13]([O:17][C:18]([F:19])([F:21])[F:20])=[CH:12][C:11]=2[Cl:22])[CH:8]=1)(=[O:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 10906Tert-Butyl nitriteHCID 193564804-Acetyl-5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethoxyphenyl)pyrazole

Produkt 1

HCID 193564794-Acetyl-3-cyano-1-(2,6-dichloro-4-trifluoromethoxyphenyl)pyrazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a stirred solution of 4-acetyl-5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethoxyphenyl)pyrazole (0.302 g) in tetrahydrofuran (10 ml) at 2° C. was added t-butylnitrite (0.66 ml). The mixture was heated under reflux for 1.5 hours and then evaporated. The residue was purified by column chromatography on silica gel eluted with dichloromethane. Combination and evaporation of suitable fractions provided the title compound as a white solid, m.p. 105.7-106.6° C.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 1.5 hours
  3. customevaporated
  4. customThe residue was purified by column chromatography on silica gel
  5. washeluted with dichloromethane
  6. customCombination and evaporation of suitable fractions

Quellen und Nachweise

ORD-Eintrag
ord-7c09078dd64c4beca4c39a7f7edeabe0
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06028096

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