반응 #974782

반응 방정식

4-methylpyrimidine

HCl

ethyl nitrite

→

titled compound

Pyrimidine-4-carbaldehyde Oxime

용매

EtOH

EtOH

반응 조건

후처리

1. 1
   workup.ADDITIONTo this white suspension was added, over 5 min
2. 2
   workup.WAITat RT for 2.5 h
3. 3
   여과The white salt was filtered
4. 4
   기타dried 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
   기타A white solid precipitated out of the purple solution
8. 8
   여과The solid was filtered
9. 9
   기타dried under vacuum

실험 절차

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.

출처