反应详情

A mixture of 30.3 parts of diethyl 2-methyl-2-[p-(2-thenoyl)phenyl]malonate and 200 parts of sodium hydroxide solution 5% is stirred and refluxed for 6 hours. The reaction mixture is allowed to cool while stirring. The whole is filtered and the aqueous phase is separated. The latter is washed with benzene, acidified with concentrated hydrochloric acid solution and stirred for 15 minutes. The product is extracted with chloroform. The extract is washed with water, dried, filtered and evaporated. The oily residue is triturated twice in petroleumether. The solid product is filtered off and crystallized twice from acetonitrile: first at -20° C and then at 0° C, yielding p-(2-thenoyl)hydratropic acid; mp. 124.3° C; also named p-(2-thenoyl)-α-methyl-phenylacetic acid.

1. temperaturerefluxed for 6 hours
2. temperatureto cool
3. stirringwhile stirring
4. filtrationThe whole is filtered
5. customthe aqueous phase is separated
6. washThe latter is washed with benzene
7. stirringstirred for 15 minutes
8. extractionThe product is extracted with chloroform
9. washThe extract is washed with water
10. customdried
11. filtrationfiltered
12. customevaporated
13. customThe oily residue is triturated twice in petroleumether
14. filtrationThe solid product is filtered off
15. customcrystallized twice from acetonitrile