反应详情

Intermediate 3 (0.066 g), EDC (0.06 g) and HOBT (0.035 g) were suspended in DMF (2 ml) and the mixture was stirred for 15 minutes. Acetic hydrazide (0.02 g) was then added and the mixture stirred under nitrogen for 18 h. Solvents were removed by concentration in vacuo and the residue partitioned between DCM and water. The layers were separated and the organic phase was washed with saturated aqueous sodium bicarbonate solution, then concentrated and applied to an SPE cartridge (aminopropyl, 1 g) which was eluted with methanol. Concentration in vacuo afforded Intermediate 4 (0.043 g). LCMS showed MH+=331; TRET=2.38 min.

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