反应详情

温度

0 °C

15 mg (0.60 mmol) of 95% sodium hydride were added at 0° C. to a solution of 116 mg (0.50 mmol) 3-methyl-4-(4-[1,2,3]triazol-1-yl-butyl)-phenol in 4.0 ml N,N-dimethylformamide and stirred for 30 min. at 0° C. 144 mg (0.50 mmol) 5-chloromethyl-2-(4-trifluoromethoxy-phenyl)-pyridine were given to the reaction mixture and stirring continued at room temperature (r.t.) overnight. After addition of 8 ml water the mixture was stirred for 1 h, the formed precipitate isolated by filtration, washed with water, methanol/water 1:1, and a small amount of ether. The residue was purified by chromatography on silica (eluent: ethyl acetate/n-heptane 4:1) to give 136 mg (56%) of the title compound as white powder.

1. stirringstirring
2. customcontinued at room temperature
3. custom(r.t.) overnight
4. stirringwas stirred for 1 h
5. customthe formed precipitate isolated by filtration
6. washwashed with water, methanol/water 1:1
7. customThe residue was purified by chromatography on silica (eluent: ethyl acetate/n-heptane 4:1)