반응 #63173

반응 방정식

ammonium chloride

isopropyl alcohol

ethyl p-nitrobenzoylacetate

→

ethyl p-aminobenzoylacetate

수율 83.1%

용매

water

반응 조건

후처리

1. 1
   온도against heat generation
2. 2
   기타to react at 70° C. for 1 hour
3. 3
   여과followed by filtration
4. 4
   workup.ADDITIONTo the filtrate was added 1 liter of water, and crystals
5. 5
   기타precipitated
6. 6
   기타were separated by filtration

실험 절차

Into a mixture comprising 224 g of reduced iron, 13.4 g of ammonium chloride, 1 liter of isopropyl alcohol and 0.2 liter of water was added 237 g of ethyl p-nitrobenzoylacetate in small portions at a temperature between 50° C. and 70° C. with caution against heat generation. The mixture was allowed to react at 70° C. for 1 hour, followed by filtration. To the filtrate was added 1 liter of water, and crystals precipitated upon cooling to 5° C. were separated by filtration to obtain 172 g of ethyl p-aminobenzoylacetate as yellow crystals having a melting point of 82° to 84° C.

출처