Hydrazine hydrate (1:1) → HCID 178515597, Verbindung

HRID 2182810Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2182810
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9](=O)[CH2:10][C:11]([O:13]C)=O.O.[NH2:17][NH2:18]>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:10]=[C:11]([OH:13])[NH:18][N:17]=1

Komponenten

4

Versuchsvorschrift

970 g of methyl 3-(2,4-dichlorophenyl)-3-oxopropionate were initially charged in 4000 ml of ethanol. Over a period of 15 min, 201 g of hydrazine hydrate were added dropwise, the mixture was stirred at room temperature overnight, the precipitated solid was filtered off and the filtrate was concentrated to ⅓ of its original volume. The filtrate was stirred for another two nights, the resulting solid was filtered off with suction and the filtrate was again concentrated to ⅓ of its original volume. This gave a total of 714.2 g (79.4%) of 3-(2,4-dichlorophenyl)-5-hydroxy-1H-pyrazole as a colorless solid. M.p.: 198° C.

Aufarbeitung

  1. filtrationthe precipitated solid was filtered off
  2. concentrationthe filtrate was concentrated
  3. stirringThe filtrate was stirred for another two nights
  4. filtrationthe resulting solid was filtered off with suction
  5. concentrationthe filtrate was again concentrated

Quellen und Nachweise

ORD-Eintrag
ord-a8803a72fbbd4cc6931c2e25f163882e
Quelldatensatz
uspto-grants-2005_05
Patentnummer
US06897322B2

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