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Hydrazine → 1H-Pyrazole-3-carboxylic acid, 5-ethyl-, ethyl ester

HRID 1360454
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1360454
O=[C:2]([CH2:8][C:9](=O)[CH2:10][CH3:11])[C:3]([O:5][CH2:6][CH3:7])=[O:4].[NH2:13][NH2:14]>C(O)(=O)C>[CH2:10]([C:9]1[NH:14][N:13]=[C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])[CH:8]=1)[CH3:11]
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Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 61590Ethyl-2,4-dioxohexanoate

Produkt 1

HCID 80276141H-Pyrazole-3-carboxylic acid, 5-ethyl-, ethyl esterAusbeute 57,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A solution of ethyl 2,4-dioxohexanoate (˜0.464 mol), prepared as described in Part A of Example 10, in glacial acetic acid (300 mL) was cooled to 0° C. Hydrazine (8.91 g, 0.278 mol) was added dropwise. The reaction was allowed to warm to ambient temperature, stirred overnight, and concentrated under reduced pressure. The residue was adjusted to pH 10 with the addition of 2 M aqueous sodium carbonate. The mixture was extracted with chloroform (3×250 mL). The combined organic layers were dried over sodium sulfate, filtered, and concentrated under reduced pressure to provide 27.0 g of ethyl 5-ethyl-1H-pyrazole-3-carboxylate, which was used without purification.

Aufarbeitung

  1. concentrationconcentrated under reduced pressure
  2. additionThe residue was adjusted to pH 10 with the addition of 2 M aqueous sodium carbonate
  3. extractionThe mixture was extracted with chloroform (3×250 mL)
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-8ffcbb7d030a4a07b665e8afb724010d
Quelldatensatz
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07879849B2

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