反应详情

温度

100 °C

Phenyl N-[2-(pyridin-2-ylmethyloxy)pyridin-5-yl] carbamate (D3, 0.20 g, 0.62 mmol) in dry dimethylformamide (10 ml) was treated with 5-trifluoromethylindoline (D6, 0.12 g, 0.62 mmol) and heated at 100° C. for 1 hour. After cooling to ambient temperature, the solvent was removed in vacuo. The residue was dissolved in dichloromethane, washed with 10% aqueous sodium hydroxide solution, dried (Na2SO4) and evaporated in vacuo. The resulting oil was chromatographed on silica gel eluting with 2% methanol/dichloromethane and triturated with diethyl ether to afford the title compound (0.08 g, 31%) as an off-white solid.

1. temperatureAfter cooling to ambient temperature
2. customthe solvent was removed in vacuo
3. dissolutionThe residue was dissolved in dichloromethane
4. washwashed with 10% aqueous sodium hydroxide solution
5. dry with materialdried (Na2SO4)
6. customevaporated in vacuo
7. customThe resulting oil was chromatographed on silica gel eluting with 2% methanol/dichloromethane
8. customtriturated with diethyl ether