Pyridine → 3-Propionylamino-pyrazine-2-carboxylic acid amide

HRID 238240

Reaktionsgleichung

Reaktionsgleichung von HRID 238240
[NH2:1][C:2]1[C:3]([C:8]([OH:10])=O)=[N:4][CH:5]=[CH:6][N:7]=1.N1C=C[CH:14]=[CH:13][CH:12]=1.[NH3:17].[OH2:18]>CN(C1C=CN=CC=1)C.C(OC(=O)CC)(=O)CC>[C:12]([NH:1][C:2]1[C:3]([C:8]([NH2:17])=[O:10])=[N:4][CH:5]=[CH:6][N:7]=1)(=[O:18])[CH2:13][CH3:14]

Komponenten

6

Edukt 3

HCID 1049PyridineHCID 726563-Amino-2-pyrazinecarboxylic acidHCID 12896473Azane;hydrate

Produkt 1

HCID 599935133-Propionylamino-pyrazine-2-carboxylic acid amideAusbeute 43 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 31263Propionic anhydrideLösungsmittel

Versuchsvorschrift

A mixture of 3-amino-pyrazine-2-carboxylic acid (20.9 g, 0.15 mol), pyridine (29.6 g, 0.375 mol) and DMAP (1.83 g, 15 mmol) in propionic acid anhydride (100 mL) was stirred at room temperature overnight. The reaction mixture was poured into NH3.H2O (500 mL) partially at 0° C. After stirred for 30 min at 0° C., the precipitated solid was filtered, washed with water, dried in air to give 3-propionylamino-pyrazine-2-carboxylic acid amide as a beige solid (12.4 g, 43%), which was used directly in the next step.

Aufarbeitung

  1. stirringAfter stirred for 30 min at 0° C.
  2. filtrationthe precipitated solid was filtered
  3. washwashed with water
  4. customdried in air

Quellen und Nachweise

ORD-Eintrag
ord-e462de6e1306463e8024cdb00ecdc717
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08642609B2

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