Hydrazine hydrate (1:1) → 3-Chloro-6-[3-(trifluoromethyl)phenoxy]-picolinic acid hydrazide

HRID 1274826Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1274826
C[O:2][C:3](=O)[C:4]1[C:9]([Cl:10])=[CH:8][CH:7]=[C:6]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)[N:5]=1.O.[NH2:24][NH2:25]>CO>[Cl:10][C:9]1[C:4]([C:3]([NH:24][NH2:25])=[O:2])=[N:5][C:6]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)=[CH:7][CH:8]=1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 539496273-Chloro-6-[3-(trifluoromethyl)phenoxy]-2-picolinic acid methyl ester

Produkt 1

HCID 702662663-Chloro-6-[3-(trifluoromethyl)phenoxy]-picolinic acid hydrazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

3-chloro-6- [3-(trifluoromethyl)phenoxy]-2-picolinic acid methyl ester (0.72 g, 0.00217 mol) was dissolved in methanol (10 ml), and then mixed with hydrazine monohydrate (1.087 g, 0.00217×10 mol). The resultant mixture was refluxed for about 3 hours. The obtained reaction solution was concentrated, and the obtained residues were distributed in ethyl acetate-saturated sodium bicarbonate water. The organic phase separated from the solution was washed with water and then dried with anhydrous sodium sulfate. After distilling off the solvent, the obtained distillation residues were purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), thereby obtaining an aimed product.

Aufarbeitung

  1. customThe obtained reaction solution
  2. concentrationwas concentrated
  3. customThe organic phase separated from the solution
  4. washwas washed with water
  5. dry with materialdried with anhydrous sodium sulfate
  6. distillationAfter distilling off the solvent
  7. distillationthe obtained distillation residues
  8. customwere purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-75954316e9554ebfbfb0f8a019c11420
Quelldatensatz
uspto-grants-2000_12
Patentnummer
US06159901

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