Potassium Acetate → HCID 19993700, Verbindung

HRID 345118Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 345118
[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]=[N:14][CH:15]([C:21]([CH2:23]Cl)=[O:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17].C([O-])(=O)C.[K+]>C(O)C>[C:16]([C:15]1[C:21]([OH:22])=[CH:23][N:13]([C:3]2[C:2]([Cl:1])=[CH:7][C:6]([C:8]([F:11])([F:10])[F:9])=[CH:5][C:4]=2[Cl:12])[N:14]=1)([O:18][CH2:19][CH3:20])=[O:17]

Komponenten

4

Edukt 2

HCID 517044Potassium AcetateHCID 19993697Ethyl 2-(2,6-dichloro-4-trifluoromethylphenylazo)-4-chloroacetoacetate

Produkt 1

HCID 19993700HCID 19993700, VerbindungAusbeute 70,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Ethyl 2-(2,6-dichloro-4-trifluoromethylphenylazo)-4-chloroacetoacetate (52.7 g) was dissolved in ethanol (650 ml) and heated to reflux. Potassium acetate (11.2 g) was added portionwise and the reaction mixture was boiled for 1 hour and allowed to cool, and the solvent was evaporated. The residue was dissolved in dichloromethane (500 ml), washed with water (2×150 ml), dried over magnesium sulfate, filtered and evaporated. The residue was triturated with hexane, filtered and dried to give 3-carboethoxy-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-hydroxypyrazole (34.0 g) as a light brown solid, m.p. 140°-143° C.

Aufarbeitung

  1. temperatureheated to reflux
  2. temperatureto cool
  3. customthe solvent was evaporated
  4. dissolutionThe residue was dissolved in dichloromethane (500 ml)
  5. washwashed with water (2×150 ml)
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was triturated with hexane
  10. filtrationfiltered
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2ae43f4a54e04108a2f91d0c6d4e15ed
Quelldatensatz
uspto-grants-1991_10
Patentnummer
US05055482

Notizen zur Reaktion

Wird geladen…