Reaktion #323178

ord-4214b87ee0c54eac8bf4a44e0e53fa72

Reaktionsgleichung

NC1=C(NC=O)C(=O)N2CCN=C2N1Cc1ccc(Cl)cc1
product
NC1=C(NC=O)C(=O)N2CCN=C2N1Cc1ccc(Cl)cc1
7-Amino-8-[(4-Chlorophenyl)Methyl]-6-(Formylamino)-2,3-Dihydroimidazo[1,2-a]Pyrimidin-5(8H)-One
CCC(=O)OC(=O)CC
propionic anhydride
CCc1nc2c([nH]1)C(=O)N1CCN=C1N2Cc1ccc(Cl)cc1
4-[(4-Chlorophenyl)Methyl]-2-Ethyl-6,7-Dihydroimidazo[1,2-a]Purin-9(4H)-One

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONA mixture of 25.00 g
  2. 2
    Temperaturat reflux for 3 hr
  3. 3
    TemperaturUpon cooling
  4. 4
    Sonstigea white solid precipitated
  5. 5
    workup.ADDITIONCH3CN was added
  6. 6
    Filtrationthe white solid filtered
  7. 7
    Sonstigeair-dried
  8. 8
    Sonstigeto give crystals, mp 278.0°-279.0° (corr.)
  9. 9
    SonstigeThe material may be recrystallized from DMF-i-PrOH

Vorschrift

A mixture of 25.00 g. (0.078 mol) of the product of Procedure 2 and 50 ml. dry pyridine in 50 ml. (0.388 mol) of propionic anhydride was heated at reflux for 3 hr. Upon cooling, a white solid precipitated. CH3CN was added, and the white solid filtered and air-dried to give crystals, mp 278.0°-279.0° (corr.). The material may be recrystallized from DMF-i-PrOH.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04642345uspto-grants-1987_02