反応 #315380

反応方程式

4-hydroxy-3-methylbenzaldehyde

K2CO3

6-chloronicotinamide

H2O

→

title compound

6-chloronicotinamide

NH4OH

収率 0.7%

溶媒

DMF

反応条件

後処理

1. 1
   その他irradiated for 5 min
2. 2
   その他Upon completion of the reaction
3. 3
   温度the mixture was cooled
4. 4
   抽出extracted with ethyl acetate
5. 5
   洗浄the combined organic layers were washed twice with water and brine
6. 6
   その他After drying the extracts
7. 7
   その他over magnesium sulfate and evaporation under vacuum the crude product
8. 8
   その他was purified by silica eel chromatography

実験手順

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.

出典