反应详情

To a solution of 5-hexenimidamide hydrochloride (P4, 200 mg) in ethanol (1.8 mL), sodium ethoxide (92 mg) was added and the mixture stirred at r.t. for 5 min. 4-(Ethyloxy)-1,1,1-trifluoro-3-buten-2-one (0.13 mL) was then added and the mixture was stirred at room temperature for 18 h. The solvent was evaporated, the residue was dissolved in dichloromethane and the organic layer was washed with H2O and dried over Na2SO4. This solution was filtered and the filtrate was concentrated in vacuo. The crude was purified by column chromatography (eluting with dichloromethane/methanol 95/5) to give 143 mg of the title compound.

1. stirringthe mixture was stirred at room temperature for 18 h
2. customThe solvent was evaporated
3. dissolutionthe residue was dissolved in dichloromethane
4. washthe organic layer was washed with H2O
5. dry with materialdried over Na2SO4
6. filtrationThis solution was filtered
7. concentrationthe filtrate was concentrated in vacuo
8. customThe crude was purified by column chromatography (eluting with dichloromethane/methanol 95/5)