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Ethyl Acetate → 1-Methylpropyl 2-(3-phenoxyphenyl)hydrazine carboxylate

HRID 379075
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 379075
[O:1]([C:8]1[CH:9]=[C:10]([NH:14][NH2:15])[CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(OCC)(=O)C.Cl[C:23]([O:25][CH:26]([CH2:28][CH3:29])[CH3:27])=[O:24]>N1C=CC=CC=1>[O:1]([C:8]1[CH:9]=[C:10]([NH:14][NH:15][C:23]([O:25][CH:26]([CH3:27])[CH2:28][CH3:29])=[O:24])[CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 8857Ethyl AcetateHCID 11829505sec-Butyl chloroformateHCID 21697795(3-Phenoxyphenyl)hydrazine

Produkt 1

HCID 216977971-Methylpropyl 2-(3-phenoxyphenyl)hydrazine carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

To 3.0 g of 3-phenoxyphenyl hydrazine, 100 ml of ethyl acetate and 2.5 ml of pyridine were added and the resultant solution was then stirred at room temperature for 30 minutes. Then, 2.5 ml of sec-butyl chloro-formate was added dropwise to the solution and stirred for 1 hour at room temperature. The solution was then washed twice, each time with 100 ml of water. After each wash, the aqueous fraction was removed from the organic (ethyl acetate) fraction. The resulting ethyl acetate fraction was then dried over anhydrous sodium sulfate, evaporated under reduced pressure, and then purified by column chromatography on silica gel, to produce 1.5 g of 1-methylpropyl 2-(3-phenoxyphenyl)hydrazine carboxylate as an oil.

Aufarbeitung

  1. washThe solution was then washed twice
  2. customAfter each wash, the aqueous fraction was removed from the organic (ethyl acetate) fraction
  3. dry with materialThe resulting ethyl acetate fraction was then dried over anhydrous sodium sulfate
  4. customevaporated under reduced pressure
  5. custompurified by column chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-3091d23f772d4576837ca4b5f6f655b4
Quelldatensatz
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06297275B1

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