تفاعل #1904034

معادلة التفاعل

4-Fluorophenylhydrazine hydrochloride

3-methyl-2-butanone

indole

→

indole

المردود 99.9%

5-fluoro indole

المردود 99.9%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   أخرىto obtain the clear solution
2. 2
   أخرىAt the end of 40 min.
3. 3
   workup.ADDITIONthe mixture was poured
4. 4
   استخلاصThe residue was extracted into ethyl acetate (100 ml×2)
5. 5
   غسيلwashed with water (100 ml×2) and ethyl acetate layer
6. 6
   تجفيفwas dried over anhydrous sodium sulfate
7. 7
   ترشيحAfter filtration, ethyl acetate
8. 8
   أخرىwas removed
9. 9
   أخرىthe residue was dried

الإجراء التجريبي

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%).

المصدر