反应详情

To a solution of 1-(trans-4-{[(5-nitro-2-{[2-(trifluoromethoxy)benzyl]amino}pyrimidin-4-yl)amino]methyl}cyclohexyl)azetidin-3-ol (100 mg, 0.20 mmol) in CH2Cl2 (25 mL) was added dropwise a solution of diethylaminosulfur trifluoride (32 μL, 0.24 mmol) in CH2Cl2 (0.5 mL) at room temperature over a period of 15 min. When the reaction was complete, the mixture was treated with saturated NaHCO3 and stirred for 5 min. The organic phase was separated and washed with water. The organic phase was dried over Na2SO4 and concentrated. The resulting residue was purified by silica gel prep TLC using 95:5 CH2Cl2:MeOH as eluent to afford 26 mg of the title compound as a pale yellow solid (26%), m/z 499.1 [M+1]+.

1. customThe organic phase was separated
2. washwashed with water
3. dry with materialThe organic phase was dried over Na2SO4
4. concentrationconcentrated
5. customThe resulting residue was purified by silica gel prep TLC