反应详情

Piperidine (0.058 mL, 0.590 mmol, 12.0 eq.) was added to a stirring mixture of Fmoc amine 19e (0.050 g, 0.0492 mmol, 1.0 eq.) in anhydrous DMF (0.8 mL) and the mixture was stirred at ambient temperature. After 20 minutes, LCMS showed reaction was completed so 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 to dryness under reduced pressure. Co-evaporation with n-hexanes afforded the product as a brown oil, and the material was not subjected to further purification (0.040 g, assumed 100%). LC/MS (1.533 min (ES+)), m/z: 928.2 [M+H]+.

1. customreaction
2. washwashed with water (3×30 mL)
3. dry with materialThe organic layer was dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated to dryness under reduced pressure
6. customCo-evaporation with n-hexanes