反应详情

温度

90 °C

A mixture of (R)-(2,2-dimethyl-1,3-dioxolan-4-yl)methyl methanesulfonate (1.08, 5.15 mmol), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (1 g, 5.15 mmol) and NaH (262 mg, 10.9 mmol) in N,N-dimethylformamide (25 mL) was heated at 90° C. for 3 hours, then allowed to cool to room temperature., quenched with water and extracted with ethyl acetate (3×). The combined organics were washed with brine, concentrated and the residue was purified by chromatography on an Analogix® Intelliflash™ purification system using a SF25-25 g column at a flow rate of 80 mL/minute, eluting with 0% to 30% ethyl acetate:hexanes over 30 minutes to give the title compound.

1. temperatureto cool to room temperature
2. custom, quenched with water
3. extractionextracted with ethyl acetate (3×)
4. washThe combined organics were washed with brine
5. concentrationconcentrated
6. customthe residue was purified by chromatography on an Analogix® Intelliflash™ purification system
7. washeluting with 0% to 30% ethyl acetate