反应 #1904034

反应方程式

4-Fluorophenylhydrazine hydrochloride

3-methyl-2-butanone

indole

→

indole

收率 99.9%

5-fluoro indole

收率 99.9%

溶剂

acetic acid

反应条件

后处理

1. 1
   其他to obtain the clear solution
2. 2
   其他At the end of 40 min.
3. 3
   workup.ADDITIONthe mixture was poured
4. 4
   萃取The residue was extracted into ethyl acetate (100 ml×2)
5. 5
   洗涤washed with water (100 ml×2) and ethyl acetate layer
6. 6
   干燥was dried over anhydrous sodium sulfate
7. 7
   过滤After filtration, ethyl acetate
8. 8
   其他was removed
9. 9
   其他the residue was dried

实验过程

A mixture containing 4-Fluorophenylhydrazine hydrochloride (5.0 g; 30.75 mmol; ALDRICH), 3-methyl-2-butanone (3.7 g; 43 mmol; ALDRICH) and acetic acid (30 ml) was stirred for 30 min. under nitrogen to obtain the clear solution. The mixture was then refluxed at 130° C. The appearance of UV-Vis Abs. Max at 255 nm and the disappearance of the peak at 282 nm confirmed the formation of the indole. At the end of 40 min. the reaction was stopped and the mixture was poured into crushed ice (100 g). The residue was extracted into ethyl acetate (100 ml×2), washed with water (100 ml×2) and ethyl acetate layer was dried over anhydrous sodium sulfate. After filtration, ethyl acetate was removed, and the residue was dried to give 4.15 g of the indole (Yield 76%).

来源