反应详情

温度

60 °C

To a solution of 9.12 g (38 mmol) of the material from Step B in 100 mL of N,N-dimethyl formamide (DMF) was added 3.1 mL (50 mmol) of iodomethane and 3.7 g (50 mmol) of lithium carbonate. The reaction mixture was heated at 60° C. for 3 hours. After cooling the reaction mixture was partitioned between dichloromethane and water. The organic layer was dried (sodium sulfate) and the solvent was removed with a rotary evaporator and then a vacuum pump. The residue was purified by MPLC with a gradient of 20-30% ethyl acetate in hexanes as eluant to afford 7.58 g of the title compound as an off-white solid.

1. temperatureAfter cooling the reaction mixture
2. customwas partitioned between dichloromethane and water
3. dry with materialThe organic layer was dried (sodium sulfate)
4. customthe solvent was removed with a rotary evaporator
5. customThe residue was purified by MPLC with a gradient of 20-30% ethyl acetate in hexanes as eluant