反应详情

Under nitrogen, (1R,2S)-ethyl 1-amino-2-vinylcyclopropanecarboxylate tosylate salt (5 g, 1 eq.) and CDI (2.7 g, 1.1 eq.) were dissolved in THF (50 mL) containing TEA (2.3 mL, 1.1 eq.). The reaction mixture was then refluxed overnight. The solvent was removed under reduced pressure. The residue was dissolved in DCM, and washed twice with water. The organic layer was dried over sodium sulfate and then concentrated. The residue was purified by chromatography on silica gel to yield compound 33 as pale yellow oil in 70% yield.

1. temperatureThe reaction mixture was then refluxed overnight
2. customThe solvent was removed under reduced pressure
3. dissolutionThe residue was dissolved in DCM
4. washwashed twice with water
5. dry with materialThe organic layer was dried over sodium sulfate
6. concentrationconcentrated
7. customThe residue was purified by chromatography on silica gel