반응 #315380

반응 방정식

4-hydroxy-3-methylbenzaldehyde

K2CO3

6-chloronicotinamide

H2O

→

title compound

6-chloronicotinamide

NH4OH

수율 0.7%

용매

DMF

반응 조건

후처리

1. 1
   기타irradiated for 5 min
2. 2
   기타Upon completion of the reaction
3. 3
   온도the mixture was cooled
4. 4
   추출extracted with ethyl acetate
5. 5
   세척the combined organic layers were washed twice with water and brine
6. 6
   기타After drying the extracts
7. 7
   기타over magnesium sulfate and evaporation under vacuum the crude product
8. 8
   기타was purified by silica eel chromatography

실험 절차

A solution of 4-hydroxy-3-methylbenzaldehyde (1.0 equiv) in DMF (0.2 M solution) was treated with K2CO3 (1.5 equiv) and 6-chloronicotinamide (1.0 equiv). The reaction mixture was placed inside the microwave oven and then irradiated for 5 min. Upon completion of the reaction, the mixture was cooled, poured into H2O and extracted with ethyl acetate, and the combined organic layers were washed twice with water and brine. After drying the extracts over magnesium sulfate and evaporation under vacuum the crude product was purified by silica eel chromatography using CHCl3:EtOH 7%:NH4OH 0.7% to afford the title compound as a solid.

출처