反应 #1121740

反应方程式

1,4-dioxane

2-(p-nitrophenyl)-5-nitrobenzofurane

hydrochloric acid

→

2-(p-aminophenyl)-5-aminobenzofurane

收率 90.0%

溶剂

water

—

mixed solvent

反应条件

后处理

1. 1
   温度the resulting mixture was refluxed
2. 2
   过滤The hot supernatant was filtered with Celite immediately
3. 3
   其他a completion of the reaction by TLC (Thin-Layer Chromatography)
4. 4
   洗涤The residual material was adequately washed with hot 1,4-dioxane
5. 5
   过滤filtered
6. 6
   浓缩concentrated by an evaporator
7. 7
   浓缩After concentration, recrystallization

实验过程

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%.

来源