反应 #155318

反应方程式

Benzhydrylidene(5-methylbenzofuran-7-yl)amine

Hydrochloric acid

sodium hydroxide

→

5-methylbenzofuran-7-ylamine

溶剂

THF

反应条件

后处理

1. 1
   萃取followed by extraction
2. 2
   洗涤The extract was sequentially washed with an aqueous saturated sodium hydrogen solution
3. 3
   干燥The organic layer was dried over magnesium sulfate
4. 4
   浓缩concentrated to dryness under reduced pressure
5. 5
   其他The residue was purified
6. 6
   浓缩The purified product was concentrated to dryness under reduced pressure

实验过程

Benzhydrylidene(5-methylbenzofuran-7-yl)amine (17.9 g, 0.57 mmol) was dissolved in THF (150 ml). 5N Hydrochloric acid (50 ml) was added thereto, followed by stirring at room temperature for 2 hours. A 5N aqueous sodium hydroxide solution (40 ml) was added to the reaction mixture, followed by extraction using ethyl acetate. The extract was sequentially washed with an aqueous saturated sodium hydrogen solution and an aqueous saturated sodium chloride solution. The organic layer was dried over magnesium sulfate and concentrated to dryness under reduced pressure. The residue was purified using silica gel column chromatography (n-hexane:ethyl acetate=50:1→10:1). The purified product was concentrated to dryness under reduced pressure, giving a dark brown oily substance of 5-methylbenzofuran-7-ylamine (2.5 g, yield: 30%).

来源