Acetic Anhydride → HCID 54463270, Verbindung

HRID 128742

Reaktionsgleichung

Reaktionsgleichung von HRID 128742
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1C=O.[CH3:11][N:12]1[CH2:18][C:16](=[O:17])[NH:15][C:13]1=[O:14].[C:19]([O-])(=O)C.[Na+].C(OC(=O)C)(=O)C>O.C(O)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:7]([CH:19]=[C:18]2[N:12]([CH3:11])[C:13](=[O:14])[NH:15][C:16]2=[O:17])[CH:8]=[CH:9][CH:10]=1

Komponenten

7

Edukt 4

HCID 7918Acetic AnhydrideHCID 86582-MethoxybenzaldehydeHCID 692171-MethylhydantoinHCID 517045Sodium Acetate

Produkt 1

HCID 54463270HCID 54463270, VerbindungAusbeute 18,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 2-methoxybenzaldehyde (3.8 g, 28 mmoles), 1-methyl hydantoin (3.0 g 26 mmoles), sodium acetate (8.4 g, 102 mmoles), acetic anhydride (10 ml), and acetic acid (40 ml) is stirred under an inert atmosphere and heated to reflux. After 24 hours the mixture is stirred into water (350 ml), stirred, and the resulting gum is isolated and washed by decantation, then crystallized from isopropanol. Recrystallization from acetonitrile gave the pure product (1.1 g), mp 195°-197° C.

Aufarbeitung

  1. temperatureheated to reflux
  2. stirringstirred
  3. customthe resulting gum is isolated
  4. washwashed by decantation
  5. customcrystallized from isopropanol
  6. customRecrystallization from acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-73efcc85ea824ec8ab3eb3c2f8ac4619
Quelldatensatz
uspto-grants-1995_11
Patentnummer
US05464856

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