N-Hydroxyacetamidine → N'-[(3,4-dimethoxy-5-nitrobenzoyl)oxy]acetamidine

HRID 274547

Reaktionsgleichung

Reaktionsgleichung von HRID 274547
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:13]=[C:14]([N+:18]([O-:20])=[O:19])[C:15]=1[O:16][CH3:17])[C:6](N1C=CN=C1)=[O:7].[C:21](=[N:24][OH:25])([NH2:23])[CH3:22]>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:13]=[C:14]([N+:18]([O-:20])=[O:19])[C:15]=1[O:16][CH3:17])[C:6]([O:25][N:24]=[C:21]([NH2:23])[CH3:22])=[O:7]

Komponenten

4

Edukt 2

HCID 30926N-HydroxyacetamidineHCID 214590201-(3,4-Dimethoxy-5-nitrobenzoyl)imidazole

Produkt 1

HCID 53789064N'-[(3,4-dimethoxy-5-nitrobenzoyl)oxy]acetamidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

10.0 g of 1-(3,4-dimethoxy-5-nitrobenzoyl)imidazole in 50 ml of dimethylformamide are treated with 6.95 g of acetamidoxime, whereupon the mixture is stirred at 70° for 1 hour. After cooling, the mixture is poured into 500 ml of ice-water and stirred for 30 minutes. The separated crystals are filtered under suction and washed with water. After crystallization from ethyl acetate there is obtained N'-[(3,4-dimethoxy-5-nitrobenzoyl)oxy]acetamidine in the form of colorless crystals of m.p. 165°-166°.

Aufarbeitung

  1. temperatureAfter cooling
  2. stirringstirred for 30 minutes
  3. filtrationThe separated crystals are filtered under suction
  4. washwashed with water
  5. customAfter crystallization from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-23d58143224d4d4fa38511ce9689b20b
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05389653

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