反应详情

To N1-(cyanomethyl)-N2-(4-{4-[4-(tert-butoxycarbonyl)piperazin-1-yl]phenyl}-1-methyl-1H-pyrazol-3-yl)leucinamide (144 mg, 0.283 mmol) in dry THF (0.5 mL) under dry nitrogen was gradually added a total of 5 equivalents of MeSO3H (100 μL, 1.42 mmol) over a period of 4 hours in portions of 1–2 equivalents at a time and the reaction mixture was stirred overnight. Aqueous sat. NaHCO3 was added carefully and the product was extracted with EtOAc (2×), dried over Na2SO4, concentrated in vacuo, and purified by flash chromatography over silica gel (NH4OH/MeOH/CH2Cl2, 1/9/90) to afford N1-(cyanomethyl)-N2-[1-methyl-4-(4-piperazin-1-ylphenyl)-1H-pyrazol-3-yl]leucinamide. MS (−ESI): 408.4 [M−1]−.

1. extractionthe product was extracted with EtOAc (2×)
2. dry with materialdried over Na2SO4
3. concentrationconcentrated in vacuo
4. custompurified by flash chromatography over silica gel (NH4OH/MeOH/CH2Cl2, 1/9/90)