反应详情

5-Cyano-1H-indole-2-carboxylic acid ethyl ester (1.71 g, 8.0 mmol) was added to a solution of ethanol (10 mL) and potassium hydroxide (2 g) and the resulting mixture heated at reflux for 1 hour. Water was added to dissolve the precipitate, and 6N HCl was added to bring the pH to 1. The mixture was cooled in an ice bath, filtered, and the resulting colorless solid washed with cold water and dried (1.51 g). A portion (1.4 g) was suspended in hot acetic acid (40 mL) and cooled giving a solid which was filtered, washed with cold ethyl acetate and dried: Yield 980 mg 70%; HPLC (60/40) 3.09 minutes (97%).

1. temperaturethe resulting mixture heated
2. temperatureat reflux for 1 hour
3. additionwas added
4. temperatureThe mixture was cooled in an ice bath
5. filtrationfiltered
6. washthe resulting colorless solid washed with cold water
7. customdried (1.51 g)
8. temperaturecooled
9. customgiving a solid which
10. filtrationwas filtered
11. washwashed with cold ethyl acetate
12. customdried
13. customHPLC (60/40) 3.09 minutes (97%)