Реакция #5145

Уравнение реакции

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

Растворители

ethyl acetate

Условия реакции

Обработка

1. 1
   ДругоеAfter removing insoluble matters from the reaction mixture
2. 2
   Фильтрацияby filtration, 200 ml of ethyl acetate and 500 ml of water
3. 3
   workup.ADDITIONwere added to the reaction mixture
4. 4
   Экстракцияthe ethyl acetate layer was extracted
5. 5
   КонцентрированиеThe ethyl acetate layer was concentrated
6. 6
   Другоеthe residue was purified by silica gel column chromatography

Методика

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).

Источник