Реакция #1960509

Уравнение реакции

4-Fluorophenylhydrazine hydrochloride

3-methyl-2-butanone

indole

→

indole

Выход 99.9%

5-fluoro Indole

Выход 99.9%

Растворители

acetic acid

Условия реакции

Обработка

1. 1
   Другоеto obtain the clear solution
2. 2
   ДругоеAt the end of 40 min.
3. 3
   workup.ADDITIONthe mixture was poured
4. 4
   ЭкстракцияThe residue was extracted into ethyl acetate (100 ml×2)
5. 5
   Промывкаwashed with water (100 ml×2) and ethyl acetate layer
6. 6
   Сушкаwas dried over anhydrous sodium sulfate
7. 7
   ФильтрацияAfter filtration, ethyl acetate
8. 8
   Другоеwas removed
9. 9
   Другоеthe residue was dried

Методика

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%).

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