반응 #5145

반응 방정식

compound ( 1-B )

2-(2-(2-(3-nitrophenoxy)ethoxy)ethoxy)ethyl methacrylate

ammonium chloride

water

isopropyl alcohol

→

2-(2-(2-(3-aminophenoxy)ethoxy)ethoxy)ethyl methacrylate

용매

ethyl acetate

반응 조건

후처리

1. 1
   기타After removing insoluble matters from the reaction mixture
2. 2
   여과by filtration, 200 ml of ethyl acetate and 500 ml of water
3. 3
   workup.ADDITIONwere added to the reaction mixture
4. 4
   추출the ethyl acetate layer was extracted
5. 5
   농축The ethyl acetate layer was concentrated
6. 6
   기타the residue was purified by silica gel column chromatography

실험 절차

A mixture of 25 g of reduced iron, 1 g of ammonium chloride, 50 ml of water, and 250 ml of isopropyl alcohol was raised to a temperature of 75° C. with stirring and after adding dropwise an ethyl acetate solution of the compound (1-B) to the aqueous solution (the mixture) over a period of one hour, the resultant mixture was further stirred for 2 hours. After removing insoluble matters from the reaction mixture by filtration, 200 ml of ethyl acetate and 500 ml of water were added to the reaction mixture and the ethyl acetate layer was extracted. The ethyl acetate layer was concentrated and the residue was purified by silica gel column chromatography using chloroform as a developing solvent to provide 15.3 g of 2-(2-(2-(3-aminophenoxy)ethoxy)ethoxy)ethyl methacrylate (1-C).

출처