反应详情

Piperidine (4 drops, excess) was added to a stirring mixture of Fmoc allylamine 15e (0.02 g, 0.0204 mmol, 1.0 eq.) in anhydrous DMF (0.25 mL) and the mixture was stirred at ambient temperature. After 30 minutes, the reaction mixture was diluted with DCM (30 mL) and washed with water (3×30 mL). The organic layer was dried over MgSO4, filtered and concentrated under reduced pressure. The crude material was dissolved in chloroform and the resulting precipitate was collected by filtration to afford the product as an orange solid (0.001 g, 7%). LC/MS (1.495 min (ES+)), m/z: 379.5 ½[M+2H]+.

1. washwashed with water (3×30 mL)
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. dissolutionThe crude material was dissolved in chloroform
6. filtrationthe resulting precipitate was collected by filtration