Ethanol → HCID 68456339, Verbindung

HRID 500529

Reaktionsgleichung

Reaktionsgleichung von HRID 500529
Cl.[CH3:2][C:3]1[CH:4]=[C:5]([NH:9][NH2:10])[CH:6]=[CH:7][CH:8]=1.C(O)C.[C:14]([OH:18])(=[O:17])[CH:15]=O>O>[C:3]1([CH3:2])[CH:8]=[CH:7][CH:6]=[C:5]([NH:9][N:10]=[CH:15][C:14]([OH:18])=[O:17])[CH:4]=1

Komponenten

5

Edukt 3

HCID 702EthanolHCID 760Glyoxylic AcidHCID 71562m-Tolylhydrazinium(1+) chloride

Produkt 1

HCID 68456339HCID 68456339, VerbindungAusbeute 69 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel3×

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

3-Methylphenylhydrazine hydrochloride (15.9 g, 100 mmol) was dissolved in water (450 mL) and ethanol (600 mL) with heating at 60° C. A solution of glyoxylic acid (9.21 g, 100 mmol) in water (100 mL) was added to the warm solution using water (3×15 mL) to rinse. The reaction mixture was stirred at 60° C. for 45 minutes and then cooled slightly and concentrated to remove ethanol. The aqueous mixture was neutralized with NaOH and then water was added (800 mL). The precipitate was filtered, washed with water (3×100 mL), washed with hexanes (100 mL) and dried to give the subtitle compound as a brown solid (12.2 g, 69%).

Aufarbeitung

  1. washto rinse
  2. temperaturecooled slightly
  3. concentrationconcentrated
  4. customto remove ethanol
  5. additionwater was added (800 mL)
  6. filtrationThe precipitate was filtered
  7. washwashed with water (3×100 mL)
  8. washwashed with hexanes (100 mL)
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-9a2a39e92d094dbda476973e38335bed
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772235B2

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