反应详情

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

1. temperatureThe mixture was heated
2. temperatureunder reflux for 1 hour
3. customevaporated to dryness
4. customThe residue was partitioned between ether (20 ml.) and water (60 ml.)
5. customThe aqueous layer was separated
6. extractionextracted with EtOAc
7. customThe organic layer was evaporated to dryness
8. customto give a gum which
9. customwas recrystallised from EtOAc/ether/acetone