反应详情

A mixture of intermediate (2) (0.005 mol) and an aqueous hydrazine solution (0.005 mol) in ethanol (30 ml) was stirred and refluxed for 2 hours. The precipitate was filtered and washed with ethanol. Water was added. The suspension was basified with NaOH and filtered over celite. Celite was washed with ethyl acetate. The filtrate was extracted with ethyl acetate. and washed with K2CO3, then with NaCl. The organic layer was separated, dried, filtered, and the solvent was evaporated. The residue was crystallized from ACN. The precipitate was filtered off and dried, yielding 2.5 g of N-[4-[(1E)-3-amino-1-propenyl]phenyl]-4′-(trifluoromethyl)-[1,1′-biphenyl]-2-carboxamide (intermediate 3; mp. 190° C.).

1. temperaturerefluxed for 2 hours
2. filtrationThe precipitate was filtered
3. washwashed with ethanol
4. additionWater was added
5. filtrationfiltered over celite
6. washCelite was washed with ethyl acetate
7. extractionThe filtrate was extracted with ethyl acetate
8. washand washed with K2CO3
9. customThe organic layer was separated
10. customdried
11. filtrationfiltered
12. customthe solvent was evaporated
13. customThe residue was crystallized from ACN
14. filtrationThe precipitate was filtered off
15. customdried