Water → 3-Chloro-6-[3-(trifluoromethyl)phenoxy] picolinic acid, (2,2.3,3,3-pentafluoropropylidene] hydrazide

HRID 1274817Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1274817
[Cl:1][C:2]1[C:3]([C:19]([NH:21][NH2:22])=[O:20])=[N:4][C:5]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=2)=[CH:6][CH:7]=1.O.[F:24][C:25]([F:32])([C:28]([F:31])([F:30])[F:29])[CH:26]=O.O>C(O)(=O)C.C(OCC)(=O)C.O>[F:24][C:25]([F:32])([C:28]([F:31])([F:30])[F:29])[CH:26]=[N:22][NH:21][C:19](=[O:20])[C:3]1[C:2]([Cl:1])=[CH:7][CH:6]=[C:5]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:16])[F:17])[CH:10]=2)[N:4]=1

Komponenten

6

Edukt 3

HCID 962WaterHCID 2776005HCID 2776005, VerbindungHCID 702662663-Chloro-6-[3-(trifluoromethyl)phenoxy]-picolinic acid hydrazide

Produkt 1

HCID 867561013-Chloro-6-[3-(trifluoromethyl)phenoxy] picolinic acid, (2,2.3,3,3-pentafluoropropylidene] hydrazide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 22728543Water ethylacetateLösungsmittel

Versuchsvorschrift

3-chloro-6-[3-(trifluoromethyl)phenoxy]-2-picolinic acid hydrazide (0.4 g, 0.0012 mol) was dissolved in 5 ml of acetic acid. The obtained solution was mixed with 2,2,3,3,3-pentafluoropropionaldehyde monohydrate (0.199 g, 0.0012×1.0 mol), and the resultant mixture was stirred at 80° C. for 3 hours. A chilled water was poured into the obtained reaction solution which was then distributed in ethyl acetate-water. The organic phase separated from the solution was washed with water and then dried with anhydrous sodium sulfate. After distilling off the solvent from the dried product, the obtained distillation residues were purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), thereby obtaining an aimed product.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-f72fea7e3bc24759abbb7b8c7b4d054e
Quelldatensatz
uspto-grants-2000_12
Patentnummer
US06159901

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