반응 #9575

반응 방정식

hydrochloric acid

Diethyl malonate

2-bromoaniline

sodium carbonate

→

N-(2-bromophenyl)malonamic acid

수율 57.3%

용매

methanol

water

반응 조건

후처리

1. 1
   기타to collect the volatiles
2. 2
   온도to cool to ambient temperature overnight
3. 3
   기타a precipitate formed
4. 4
   기타The precipitate was isolated by filtration
5. 5
   온도The mixture was heated
6. 6
   온도at reflux for two hours
7. 7
   온도to cool to ambient temperature
8. 8
   온도cooled to 0° C
9. 9
   기타a white precipitate formed
10. 10
    기타The precipitate was isolated by filtration
11. 11
    세척washed with water
12. 12
    기타dried overnight on the filter funnel

실험 절차

Diethyl malonate (101 mL, 0.989 mol) and 2-bromoaniline (50.g, 0.291 mol) were combined and heated at 180° C. for six hours. A Dean-Stark trap was used to collect the volatiles. The reaction was allowed to cool to ambient temperature overnight; a precipitate formed. The precipitate was isolated by filtration and combined with methanol (160 mL), water (800 mL), and solid sodium carbonate (105 g). The mixture was heated at reflux for two hours, allowed to cool to ambient temperature, and then cooled to 0° C. The mixture was adjusted to pH 2 with the addition of 3 N hydrochloric acid; a white precipitate formed. The precipitate was isolated by filtration, washed with water, and dried overnight on the filter funnel to provide 43 g of N-(2-bromophenyl)malonamic acid as a white solid.

출처