반응 #1960509

반응 방정식

4-Fluorophenylhydrazine hydrochloride

3-methyl-2-butanone

indole

→

indole

수율 99.9%

5-fluoro Indole

수율 99.9%

용매

acetic acid

반응 조건

후처리

1. 1
   기타to obtain the clear solution
2. 2
   기타At the end of 40 min.
3. 3
   workup.ADDITIONthe mixture was poured
4. 4
   추출The residue was extracted into ethyl acetate (100 ml×2)
5. 5
   세척washed with water (100 ml×2) and ethyl acetate layer
6. 6
   건조was dried over anhydrous sodium sulfate
7. 7
   여과After filtration, ethyl acetate
8. 8
   기타was removed
9. 9
   기타the residue was dried

실험 절차

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%).

출처