反应详情

温度

0 °C

36 mg (0.90 mmol) of 95% sodium hydride were added to at 0° C. to a solution of 173 mg (0.75 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. 214 mg (0.75 mmol) 3-chloromethyl-2-methyl-6-(4-trifluoromethyl-phenyl)-pyridine (WO 2005/049573) 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, water/methanol 1:1, and ether. The residue was purified by chromatography on silica (eluent: ethyl acetate) to yield 227 mg (63%) of the title compound as white crystals.

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, water/methanol 1:1, and ether
7. customThe residue was purified by chromatography on silica (eluent: ethyl acetate)