反応 #1960509

反応方程式

4-Fluorophenylhydrazine hydrochloride

3-methyl-2-butanone

indole

→

indole

収率 99.9%

5-fluoro Indole

収率 99.9%

溶媒

acetic acid

反応条件

後処理

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

実験手順

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%).

出典