反应详情

To 400 parts of liquid ammonia are added a trace of ferric chloride and 3 parts of sodium. The mixture is stirred for 30 minutes, after which 14.8 parts of 2-[p-(2-thenoyl)phenyl]acetic acid are added slowly during 30 minutes, and the mixture is further stirred for 45 minutes. 13.6 parts of methyl iodide are added dropwise and the reaction mixture is stirred for 2h. 30 400 parts of diethyl ether are then added and the mixture is stirred overnight. The ammonia is evaporated and the resulting solution is acidified with diluted hydrochloric acid. The ethereal layer is separated and extracted with 10% sodium hydroxide solution. The extract is washed with ether, acidified and extracted with ether. The ethereal solution is dried on sodium sulfate and the ether is evaporated in vacuo. The residue is triturated in petroleumether, filtered off and crystallized twice from acetonitrile, first at -20° C and then at 0° C, yielding p-(2-thenoyl)hydratropic acid.

1. stirringthe mixture is further stirred for 45 minutes
2. stirringthe reaction mixture is stirred for 2h
3. stirringthe mixture is stirred overnight
4. customThe ammonia is evaporated
5. customThe ethereal layer is separated
6. extractionextracted with 10% sodium hydroxide solution
7. washThe extract is washed with ether
8. extractionextracted with ether
9. customThe ethereal solution is dried on sodium sulfate
10. customthe ether is evaporated in vacuo
11. customThe residue is triturated in petroleumether
12. filtrationfiltered off
13. customcrystallized twice from acetonitrile, first at -20° C