Methyl acetoacetate → HCID 178463089, Verbindung

HRID 350875

Reaktionsgleichung

Reaktionsgleichung von HRID 350875
C(O)(=O)C(O)=O.[CH2:7]([NH:9][NH2:10])[CH3:8].C(N(CC)CC)C.[C:18](OC)(=[O:23])[CH2:19][C:20]([CH3:22])=O>C1(C)C=CC=CC=1>[CH2:7]([N:9]1[C:18]([OH:23])=[CH:19][C:20]([CH3:22])=[N:10]1)[CH3:8]

Komponenten

5

Edukt 3

HCID 7757Methyl acetoacetateHCID 8471TriethylamineHCID 96181Hydrazine, ethyl-, ethanedioate (1:1)

Produkt 1

HCID 178463089HCID 178463089, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A suspension of 3.9 g of ethyl hydrazine oxalate and 3.6 ml of triethylamine in 80 ml of toluene was stirred at room temperature for 15 min. 2.8 ml of methyl acetoacetate was added and the mixture was azeotroped for 1.5 h. The mixture was evaporated and the residue was purified by flash chromatography on silica gel using dichloromethane/methanol (97:3) for the elution to give 3.1 g of 2-ethyl-5-methyl-2H-pyrazol-3-ol as an orange solid.

Aufarbeitung

  1. customthe mixture was azeotroped for 1.5 h
  2. customThe mixture was evaporated
  3. customthe residue was purified by flash chromatography on silica gel
  4. washfor the elution

Quellen und Nachweise

ORD-Eintrag
ord-6d1a392d47f548fd945ce90ac47d6138
Quelldatensatz
uspto-grants-2007_02
Patentnummer
US07183296B2

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