Water → HCID 136359197, Verbindung

HRID 1155541Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1155541
Cl.[NH2:2][OH:3].O.[OH-].[Na+].[CH2:7]([NH:9][C:10]1[CH:15]=[C:14]([C:16](=O)[CH3:17])[CH:13]=[CH:12][N:11]=1)[CH3:8]>CO>[CH2:7]([NH:9][C:10]1[CH:15]=[C:14]([C:16](=[N:2][OH:3])[CH3:17])[CH:13]=[CH:12][N:11]=1)[CH3:8]

Komponenten

6

Edukt 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 131452661-(2-Ethylamino-4-pyridyl)-1-ethanone

Produkt 1

HCID 136359197HCID 136359197, VerbindungAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a mixture of 7 g. (0.1 mole) of hydroxylamine hydrochloride in 40 ml. of water and 50 ml. of 2 N sodium hydroxide was added 11.5 g. (70 mmoles) of 1-(2-ethylamino-4-pyridyl)-1-ethanone, and the resulting mixture heated to boiling. Methanol was carefully added until the mixture became homogeneous. Heating was continued until the mixture became cloudy. The mixture was cooled and the resulting precipitate filtered, washed with water and dried. Recrystallization from toluene gave 10.9 g. (87%) of the desired product, m.p. 155°-156° C.

Aufarbeitung

  1. additionTo a mixture of 7 g
  2. temperatureHeating
  3. temperatureThe mixture was cooled
  4. filtrationthe resulting precipitate filtered
  5. washwashed with water
  6. customdried
  7. customRecrystallization from toluene
  8. customgave 10.9 g

Quellen und Nachweise

ORD-Eintrag
ord-326e57327d40407a9207cc1b20120c85
Quelldatensatz
uspto-grants-1981_11
Patentnummer
US04302464

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