反应详情

To a solution of 1-{[(4R)-2,2-dimethyl-1,3-dioxolan-4-yl]methyl}-4-iodo-5-methyl-1H-pyrazole (67.0 mg, 0.208 mmol) in THF (2 mL, 20 mmol) at rt was added 1.3 M of isopropylmagnesium chloride in THF (0.64 mL, 0.83 mmol), and the mixture was stirred for 1 h. The reaction was quenched with 2-methoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (0.1704 mL, 1.040 mmol), and allowed to stir at rt for 1 h. Sat. NH4Cl was added, and the organic solvent was removed in vacuo. The material was extracted with DCM and water. The organic layer was concentrated in vacuo to afford the title compound as a clear oil. MS (ES+): m/z=322.21/323.20/324.22 (50/100/50) [MH+]. HPLC: tR=1.49 min (polar—3 min, UPLC-ACQUITY).

1. stirringto stir at rt for 1 h
2. customthe organic solvent was removed in vacuo
3. extractionThe material was extracted with DCM and water
4. concentrationThe organic layer was concentrated in vacuo