反应详情

3-Methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (7.4 g, 0.0356 mol), 1,1′,1″-(chloromethanetriyl)tribenzene (9.9 g, 0.0356 mol) and triethylamine (7.2 g, 0.0712 mol) were suspended in N,N-dimethylformamide (70.0 mL) and stirred at room temperature for 16 hours. The reaction mixture was quenched by addition of water (30.0 mL) and extracted with ethyl acetate (3×30.0 mL). The combined organic layers were washed with saturated aqueous sodium chloride solution (40.0 mL), dried over sodium sulfate and concentrated in vacuo. This crude residue was initially purified via column chromatography eluting with petroleum ether:ethyl acetate (10:1, by volume) and then purified by preparative HPLC to yield title compound as a white solid.

1. customThe reaction mixture was quenched by addition of water (30.0 mL)
2. extractionextracted with ethyl acetate (3×30.0 mL)
3. washThe combined organic layers were washed with saturated aqueous sodium chloride solution (40.0 mL)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThis crude residue was initially purified via column chromatography
7. washeluting with petroleum ether:ethyl acetate (10:1, by volume)
8. custompurified by preparative HPLC