反应详情

A mixture of intermediate (16) (0.048 mol) in DCM (200 ml) was cooled on an ice bath. 3-chloro-3-oxo-propanoic acid, ethyl ester (0.105 mol) was added dropwise. The mixture was stirred at a low temperature for 30 min, then stirred and refluxed for 1 hour and poured out into water. The organic layer was separated, washed with K2CO3 10%, dried (MgSO4), filtered and the solvent was evaporated till dryness. The product was used without further purification, yielding (quant.) N-[2-(3-chlorobenzoyl)-4-[(4-phenyl-2-thiazolyl)carbonyl]phenyl]-3-oxo-β-alanine ethyl ester (intermediate 17).

1. temperaturewas cooled on an ice bath
2. stirringstirred
3. temperaturerefluxed for 1 hour
4. customThe organic layer was separated
5. washwashed with K2CO3 10%
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customthe solvent was evaporated till dryness
9. customThe product was used without further purification