Reaktion #974782

Reaktionsgleichung

4-methylpyrimidine

HCl

ethyl nitrite

→

titled compound

Pyrimidine-4-carbaldehyde Oxime

Lösungsmittel

EtOH

EtOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONTo this white suspension was added, over 5 min
2. 2
   workup.WAITat RT for 2.5 h
3. 3
   FiltrationThe white salt was filtered
4. 4
   Sonstigedried under vacuum
5. 5
   workup.DISSOLUTIONThe salt was dissolved into 20 ml H2O
6. 6
   workup.ADDITIONvery slowly treated with about 200 ml saturated aqueous KHCO3
7. 7
   SonstigeA white solid precipitated out of the purple solution
8. 8
   FiltrationThe solid was filtered
9. 9
   Sonstigedried under vacuum

Vorschrift

9.14 g (97.11 mmol) of 4-methylpyrimidine was slowly added to a 0° C. solution of 8.75 g HCl in 40 ml EtOH. To this white suspension was added, over 5 min, 61 ml of a 10-20% by weight solution of ethyl nitrite in EtOH. The reaction was stirred at 0° C. for 10 min and then at RT for 2.5 h. The white salt was filtered and dried under vacuum. The salt was dissolved into 20 ml H2O and very slowly treated with about 200 ml saturated aqueous KHCO3. A white solid precipitated out of the purple solution. The solid was filtered and dried under vacuum to yield the titled compound.

Quelle