反应详情

A mixture of 4.2 parts of 2-[2-chloro-3-(2-thenoyl)phenyl]acetonitrile, 7 parts of acetic acid, 7 parts of water and 12 parts of sulfuric acid is stirred and boiled for 1h. 30. The reaction mixture is cooled, poured onto water and extracted with ether. The extract is washed with water, extracted with 50 parts of a 5% sodium hydroxide solution and the alkaline solution is washed with ether. After acidification with diluted hydrochloric acid solution, the whole is extracted again with ether. The extract is washed with water, treated with charcoal, filtered and evaporated. The residue is purified by column-chromatography over silicagel, using a mixture of chloroform and 5% of methanol as eluent. The pure fractions are collected and the eluent is evaporated, yielding 2-[2-chloro-3-(2-thenoyl)phenyl]acetic acid; mp. 112.2° C.

1. temperatureThe reaction mixture is cooled
2. additionpoured onto water
3. extractionextracted with ether
4. washThe extract is washed with water
5. extractionextracted with 50 parts of a 5% sodium hydroxide solution
6. washthe alkaline solution is washed with ether
7. extractionAfter acidification with diluted hydrochloric acid solution, the whole is extracted again with ether
8. washThe extract is washed with water
9. additiontreated with charcoal
10. filtrationfiltered
11. customevaporated
12. customThe residue is purified by column-chromatography over silicagel
13. additiona mixture of chloroform and 5% of methanol as eluent
14. customThe pure fractions are collected
15. customthe eluent is evaporated