Water → HCID 14986264, Verbindung

HRID 2248756Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2248756
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][CH2:11][CH3:12])[C:3]=1[C:4]#[N:5].N1C=CC=CC=1.[C:19]([O:23][CH2:24][C:25](Cl)=[O:26])(=[O:22])[CH2:20][CH3:21].O>C(Cl)Cl>[CH2:11]([NH:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:2]([NH:1][C:25](=[O:26])[CH2:24][O:23][C:19](=[O:22])[CH2:20][CH3:21])[C:3]=1[C:4]#[N:5])[CH3:12]

Komponenten

6

Versuchsvorschrift

To a solution of 2-amino-6-(ethylamino)benzonitrile (2.3 g) in methylene chloride (50 ml) is added pyridine (1.6 ml), and thereto is added dropwise propionyloxyacetyl chloride (3.0 ml) which is cooled in an ice bath. The mixture is stirred at room temperature for 1 hour, and thereafter, water is added thereto, and the mixture is extracted with methylene chloride. The organic layer is dried over anhydrous sodium sulfate, and the solvent is distilled off under reduced pressure. The resulting crude crystals are recrystallized from ethanol to give the title compound (1.6 g) having the following physical properties.

Aufarbeitung

  1. temperatureis cooled in an ice bath
  2. extractionthe mixture is extracted with methylene chloride
  3. dry with materialThe organic layer is dried over anhydrous sodium sulfate
  4. distillationthe solvent is distilled off under reduced pressure
  5. customThe resulting crude crystals are recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-c037378908494ffbbffa2ae2d5695fcf
Quelldatensatz
uspto-grants-1991_08
Patentnummer
US05041462

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