反应详情

1-methyl-1H-pyrrolo[2,3-c]pyridine-3-carbaldehyde (WO 05066132) (6.5 g, 40.6 mmol) was dissolved in a mixture solvent of THF (120 mL) and t-butyl alcohol (40 mL) under nitrogen. A 2M 2-methyl-2-butene solution in THF (120 mL, 46 mmol) was added followed by a solution of NaClO2 (11.02 g, 122 mmol) and NaH2PO4 (21.9 g, 183 mmol) in water (30 mL). The reaction mixture was stirred at room temperature overnight under nitrogen. The reaction mixture was concentrated in vacuo to remove organic solvents, and the residue was filtered. The precipitate contained the title compound as white solid in 57% yield, 4.1 g.

1. concentrationThe reaction mixture was concentrated in vacuo
2. customto remove organic solvents
3. filtrationthe residue was filtered