反应详情

As shown in step 6-i of Scheme 6, to a mixture of 5-bromo-2-fluoro-pyrimidine (1 g, 5.651 mmol) in iPrOH (10 mL) was added TEA (1.143 g, 1.574 mL, 11.30 mmol) and trans-4-aminocyclohexan-1-ol (650.8 mg, 5.651 mmol). The mixture was microwaved for 20 min at 150° C., concentrated under reduced pressure, diluted with EtOAc, washed with water, and dried over Na2SO4. After removal of the volatiles under reduced pressure, the residue was purified by medium pressure silica gel chromatography (0-80% EtOAc/hexanes gradient) to provide (trans)-4-((5-bromopyrimidin-2-yl)amino)cyclohexanol (compound 1013, 1.2 g): 1H-NMR (300 MHz, CDCl3) δ 8.28 (s, 2H), 5.03 (d, J=8.1 Hz, 1H), 3.91-3.49 (m, 2H), 2.31-1.90 (m, 4H), 1.56-1.19 (m, 4H).

1. customThe mixture was microwaved for 20 min at 150° C.
2. concentrationconcentrated under reduced pressure
3. additiondiluted with EtOAc
4. washwashed with water
5. dry with materialdried over Na2SO4
6. customAfter removal of the volatiles under reduced pressure
7. customthe residue was purified by medium pressure silica gel chromatography (0-80% EtOAc/hexanes gradient)