反应详情

To a solution of methyl 7-chloro-6-oxoheptanoate (2.0 g.) in hot EtOH (20 ml.) was added a solution of 2,2,2-trifluoroethylamidinothiourea (2.1 g.) in hot EtOH (20 ml.). The resulting mixture was heated under reflux for 1 hour. The mixture was then evaporated to dryness and the residue partitioned between ether (20 ml.) and water (60 ml.). The aqueous layer was separated and basified with sodium bicarbonate and extracted with EtOAc. The EtOAc solution was evaporated to dryness and the residue crystallised from EtOAc/ether containing a small amount of acetone to give methyl 5-[2-(2-[2,2,2-trifluoroethyl]guanidino)thiazol-4-yl]valerate which was used without further purification.

1. temperatureThe resulting mixture was heated
2. temperatureunder reflux for 1 hour
3. customThe mixture was then evaporated to dryness
4. customthe residue partitioned between ether (20 ml.) and water (60 ml.)
5. customThe aqueous layer was separated
6. extractionextracted with EtOAc
7. customThe EtOAc solution was evaporated to dryness
8. customthe residue crystallised from EtOAc/ether containing a small amount of acetone