反応 #66717

反応方程式

ammonium formate

ammonium formate

N-[4-(1-Hydroxy-1-methyl-ethyl)-3-methoxy-phenyl]-acetamide

ammonium formate

→

N-(4-Isopropyl-3-methoxy-phenyl)-acetamide

収率 99.2%

溶媒

acetic acid

反応条件

後処理

1. 1
   温度The reaction mixture was heated to reflux
2. 2
   温度Reflux
3. 3
   workup.WAITwas continued for another hour
4. 4
   温度the reaction mixture was cooled
5. 5
   ろ過filtered through Celite
6. 6
   workup.ADDITIONThe filtrate was diluted with water
7. 7
   抽出extracted with EtOAc
8. 8
   洗浄the combined organic layers were washed with brine
9. 9
   乾燥dried over magnesium sulfate
10. 10
    その他Evaporation under reduced pressure

実験手順

N-[4-(1-Hydroxy-1-methyl-ethyl)-3-methoxy-phenyl]-acetamide (16.4 g) in 100 ml glacial acetic acid was stirred at room temperature under N2, and palladium on activated carbon (3 g 10 Wt %) was added, followed by 5 g of ammonium formate. The reaction mixture was heated to reflux. After 30 minutes 5 g ammonium formate was added, and after 45 minutes another 8.5 g ammonium formate was added. Reflux was continued for another hour, then the reaction mixture was cooled, and filtered through Celite. The filtrate was diluted with water, extracted with EtOAc, and the combined organic layers were washed with brine and dried over magnesium sulfate. Evaporation under reduced pressure gave N-(4-Isopropyl-3-methoxy-phenyl)-acetamide (15.1 g, 99%).

出典