反应详情

To a solution of 2-bromo-6-methylaniline (0.5 g, 2.69 mmol) in acetonitrile (30.0 mL) at ambient temperature was added a 37% aqueous solution of formaldehyde (4.0 mL, 53.6 mmol), followed by NaBH3CN (1.40 g, 22.1 mmol). The pH of the reaction was adjusted to pH 5-6 with glacial acetic acid, and the reaction was stirred for 4 h, then the solvent was removed. The residue was dissolved in EtOAc, and basified with NaOH 2N, dried over MgSO4, and filtered. The solvent was removed, and the residue was purified by silica gel flash chromatography with EtOAc (15%) and hexanes (85%) as eluent to produce Compound 150 as a clear oil.

1. customthe solvent was removed
2. dissolutionThe residue was dissolved in EtOAc
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customThe solvent was removed
6. customthe residue was purified by silica gel flash chromatography with EtOAc (15%) and hexanes (85%) as eluent