反应详情

Intermediate 3 (0.060 g), EDC (0.06 g) and HOBT (0.035 g) were suspended in DMF (2 ml) and stirred under nitrogen for 15 minutes. Isobutyric acid hydrazide (0.027 g) was then added and the mixture stirred under nitrogen for 18 h. Solvents were removed in vacuo and the residue partitioned between DCM and water. The organic phase was washed with saturated aqueous sodium bicarbonate solution, then concentrated in vacuo and applied to an SPE cartridge (aminopropyl, 1 g) which was eluted with methanol. Concentration in vacuo afforded Intermediate 10. LCMS showed MH+=359; TRET=2.70 min.

1. stirringthe mixture stirred under nitrogen for 18 h
2. customSolvents were removed in vacuo
3. customthe residue partitioned between DCM and water
4. washThe organic phase was washed with saturated aqueous sodium bicarbonate solution
5. concentrationconcentrated in vacuo
6. washwas eluted with methanol
7. concentrationConcentration in vacuo