Nitric Acid → HCID 19737188, Verbindung

HRID 258258Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 258258
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[N:13]1[C:21]2[C:16](=[CH:17][CH:18]=[C:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:20]=2)[CH:15]=[N:14]1.[N+:27]([O-])([OH:29])=[O:28]>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[N:13]1[C:21]2[C:16](=[CH:17][C:18]([N+:27]([O-:29])=[O:28])=[C:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:20]=2)[CH:15]=[N:14]1

Komponenten

4

Edukt 2

HCID 944Nitric AcidHCID 19737207HCID 19737207, Verbindung

Produkt 1

HCID 19737188HCID 19737188, VerbindungAusbeute 63 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

To a solution of ethyl 1-(2,6-dichloro-4-trifluoromethylphenyl)indazol-6-yl carboxylate [Compound No. 62] (3 g) in conc. sulfuric acid (20 g), fuming nitric acid (0.7 g) was added dropwise while cooling with ice, and the resultant mixture was stirred at room temperature for 3 hours. After completion of the reaction, the reaction mixture was poured into ice water, and the precipitated crystals were collected by filtration, washed and dried. The crystals were purified by silica gel column chromatography with hexane-ethyl acetate (4:1) to give ethyl 1-(2,6-dichloro-4-trifluoromethylphenyl)-5-nitroindazol-6-yl carboxylate (2.1 g).

Aufarbeitung

  1. temperaturewhile cooling with ice
  2. customAfter completion of the reaction
  3. filtrationthe precipitated crystals were collected by filtration
  4. washwashed
  5. customdried
  6. customThe crystals were purified by silica gel column chromatography with hexane-ethyl acetate (4:1)

Quellen und Nachweise

ORD-Eintrag
ord-c6be27b2517f4588ab22ee19158d1701
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05266556

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