反应详情

温度

0 °C

{6-[5-(3-Trifluoromethoxy-phenyl)-pent-4-ynoylamino]-indol-1-yl}-acetic acid ethyl ester (50 mg, 0.11 mmol) was added to a suspension of sodium hydride (9 mg, 0.22 mmol) in tetrahydrofuran (1.5 ml) at 0° C. The mixture was stirred for 30 min at 0° C., methyl iodide (30 μl, 0.44 mmol) was added and stirring was continued for 14 h at ambient temperature. The suspension was cooled to 0° C., sodium hydride (13 mg, 0.33 mmol) and methyl iodide (45 μl, 0.66 mmol) were added and the mixture was stirred for 4 h at ambient temperature. Ethyl acetate was added, the solution was successively washed with brine, 1 N HCl/ice water 1/1 and brine and dried over sodium sulfate. The solvent was removed under reduced pressure to give 42 mg (0.09 mmol, 82%) of the title compound as yellow solid.

1. stirringstirring
2. waitwas continued for 14 h at ambient temperature
3. temperatureThe suspension was cooled to 0° C.
4. stirringthe mixture was stirred for 4 h at ambient temperature
5. washthe solution was successively washed with brine, 1 N HCl/ice water 1/1 and brine
6. dry with materialdried over sodium sulfate
7. customThe solvent was removed under reduced pressure