反应详情

温度

70 °C

To a solution of the above (4-chloro-5-trifluoromethyl-pyrimidin-2-yl)-(2-trifluoromethoxy-benzyl)-amine (80 mg, 0.22 mmol) in DMF (2 mL) was added the Boc-protected cyclohexyl amine (74 mg, 0.33 mmol) followed by DIPEA (37 μL, 0.22 mmol). The reaction mixture was stirred at 70° C. for 3 h. When the reaction was complete, the reaction mixture was diluted with EtOAc and washed with water (×4). The organic phase was dried over anhydrous Na2SO4 and concentrated in vacuo. The resulting residue was purified by silica gel preparative TLC using 95:5 CH2Cl2:MeOH as an eluent. The resulting residue was then re-dissolved in CH2Cl2 (10 mL) and TFA (1 mL) was added. The reaction mixture was stirred at room temperature for 2 h and treated with saturated NaHCO3. The product was extracted with CH2Cl2 and dried over anhydrous Na2SO4. Silica gel preparative TLC using CH2Cl2:MeOH:NH4OH 10:1:0.2 as an eluent afforded 56 mg (56%) of the title compound as a white solid, m/z 462.4 [M−1]+.

1. washwashed with water (×4)
2. dry with materialThe organic phase was dried over anhydrous Na2SO4
3. concentrationconcentrated in vacuo
4. customThe resulting residue was purified by silica gel preparative TLC
5. dissolutionThe resulting residue was then re-dissolved in CH2Cl2 (10 mL)
6. additionTFA (1 mL) was added
7. stirringThe reaction mixture was stirred at room temperature for 2 h
8. additiontreated with saturated NaHCO3
9. extractionThe product was extracted with CH2Cl2
10. dry with materialdried over anhydrous Na2SO4