Toluene → 2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetohydrazide

HRID 335464

Reaktionsgleichung

Reaktionsgleichung von HRID 335464
[CH2:1]([C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH2:10][CH3:11])[C:4]=1[C:12](=[O:18])[C:13](OCC)=[O:14])[CH3:2].C1(C)C=CC=CC=1.O.[NH2:27][NH2:28]>O>[CH2:1]([C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH2:10][CH3:11])[C:4]=1[C:12](=[O:18])[C:13]([NH:27][NH2:28])=[O:14])[CH3:2]

Komponenten

5

Edukt 3

HCID 1140TolueneHCID 24654Hydrazine hydrate (1:1)HCID 56942718Ethyl (2,6-diethyl-4-methylphenyl)glyoxylate

Produkt 1

HCID 569428732-(2,6-Diethyl-4-methylphenyl)-2-oxoacetohydrazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

To a 100 mL volume three-necked flask, ethyl 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetate ((9-a) (10.0 g)) and toluene (35 ml) were added. Hydrazine hydrate (2.13 ml) was added dropwise thereto at 60° C. and the obtained mixture was stirred at 70° C. for 7 hours. The reaction mixture was cooled to room temperature, water was added thereto and the organic layer was removed. The aqueous layer was extracted with toluene. The organic layers were combined and concentrated under reduced pressure to give 9.40 g of 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetohydrazide ((12-1)-(11)-39).

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customthe organic layer was removed
  3. extractionThe aqueous layer was extracted with toluene
  4. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-cd240b7a84414d0a9629b9b3cbb75b72
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08884010B2

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