反应详情

温度

90 °C

To 4-methoxybenzyl N-[4-bromo-1-(tert-butoxycarbonyl)-1H-pyrazol-3-yl]leucinate (1.45 g, 2.92 mmol), 4-[4-(tert-butoxycarbonyl)-1-piperazinyl]phenylboronic acid (1.117 g, 3.65 mmol, prepared as described in Example 1) and catalyst PdCl2(dppf) (75 mg, 0.09 mmol) in DMF (30 mL) under dry nitrogen was added aqueous sodium carbonate (2.0 M, 3.3 mL, 6.6 mmol). The reaction was heated to 90° C. for 0.5 hour and an additional aliquot of PdCl2(dppf) (20 mg, 0.022 mmol) was added and the reaction mixture was heated for 1½ hour. Water was added and the product extracted with ether (2×), dried over Na2SO4, concentrated in vacuo, and purified by flash chromatography over silica gel (EtOAc/Hex, 25/75) to afford 4-methoxybenzyl N-(1-(tert-butoxycarbonyl)-4-{4-[4-(tert-butoxycarbonyl)piperazin-1-yl]phenyl}-1H-pyrazol-3-yl)leucinate.

1. temperaturethe reaction mixture was heated for 1½ hour
2. extractionthe product extracted with ether (2×)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated in vacuo
5. custompurified by flash chromatography over silica gel (EtOAc/Hex, 25/75)