反应详情

To a solution of 2-chloro-9-cyclohexyl-7-fluoro-7-methyl-8,9-dihydro-5H-pyrimido[4,5-b][1,4]diazepin-6(7H)-one (313 mg, 2.85 mmol) in 10 mL of DMA was added sodium hydride (60% dispersion in mineral oil, 44 mg, 1.1 mmol) at 0° C., followed by the dropwise addition of methyl iodide (0.07 mL, 1.1 mmol). The reaction mixture was warmed up to rt and stirred for 1 h. The whole was poured into ice-water, extracted with ethyl acetate. The organic layer was washed with brine and dried over Na2SO4. The solution was concentrated in vacuo and used for next step reaction (330 mg). [M+H] calc'd for C15H20ClFN4O, 327; found 327.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over Na2SO4
4. concentrationThe solution was concentrated in vacuo
5. customused for next step reaction (330 mg)