반응 #1121740

반응 방정식

1,4-dioxane

2-(p-nitrophenyl)-5-nitrobenzofurane

hydrochloric acid

→

2-(p-aminophenyl)-5-aminobenzofurane

수율 90.0%

용매

water

—

mixed solvent

반응 조건

후처리

1. 1
   온도the resulting mixture was refluxed
2. 2
   여과The hot supernatant was filtered with Celite immediately
3. 3
   기타a completion of the reaction by TLC (Thin-Layer Chromatography)
4. 4
   세척The residual material was adequately washed with hot 1,4-dioxane
5. 5
   여과filtered
6. 6
   농축concentrated by an evaporator
7. 7
   농축After concentration, recrystallization

실험 절차

Then, 12.42 g (1.0 equivalent) of the obtained 2-(p-nitrophenyl)-5-nitrobenzofurane was added to 48.85 g (20.0 equivalents) of a 100 mesh iron powder previously activated by 0.5 ml of concentrated hydrochloric acid in 150 ml of a mixed solvent of 1,4-dioxane and water in proportions of 1:1, and the resulting mixture was refluxed by heating at about 110° C. for 2 hours and heavily stirred. The hot supernatant was filtered with Celite immediately after confirming a completion of the reaction by TLC (Thin-Layer Chromatography). The residual material was adequately washed with hot 1,4-dioxane and filtered. This operation was repeated three or four times, and then filtrates were combined and concentrated by an evaporator. After concentration, recrystallization was carried out with ethanol to obtain 7.1 g of orange-colored 2-(p-aminophenyl)-5-aminobenzofurane (amino compound A) at an yield of 90%.

출처