反应详情

1-Chloroethyl chloroformate (0.078 mol) was added dropwise to a stirring mixture of intermediate (20) (0.039 mol) in 1,2-dichloro-ethane (500 ml). The mixture was stirred for 30 minutes and then stirred and refluxed overnight. The solvent was evaporated. Methanol (500 ml) was added. The mixture was stirred and refluxed overnight. The solvent was evaporated. The residue was triturated in DIPE. The precipitate was filtered off and dried, yielding 20.8 g of N-[4-(1,2,3,6-tetrahydro-4-pyridinyl)phenyl]-4′-(trifluoro-methyl )-[1,1′-biphenyl]-2-carboxamide (intermediate 21).

1. stirringstirred
2. temperaturerefluxed overnight
3. customThe solvent was evaporated
4. additionMethanol (500 ml) was added
5. stirringThe mixture was stirred
6. temperaturerefluxed overnight
7. customThe solvent was evaporated
8. customThe residue was triturated in DIPE
9. filtrationThe precipitate was filtered off
10. customdried