반응 #169036

반응 방정식

ammonium formate

ammonium formate

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

ammonium formate

→

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

수율 99.2%

용매

acetic acid

반응 조건

후처리

1. 1
   온도The reaction mixture was heated to reflux
2. 2
   온도Reflux
3. 3
   workup.WAITwas continued for another hour
4. 4
   온도the reaction mixture was cooled
5. 5
   여과filtered through Celite
6. 6
   workup.ADDITIONThe filtrate was diluted with water
7. 7
   추출extracted with EtOAc
8. 8
   세척the combined organic layers were washed with brine
9. 9
   건조dried over magnesium sulfate
10. 10
    기타Evaporation under reduced pressure

실험 절차

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%).

출처