反应详情

To a solution of 2-{4-[3,5-dimethyl-4-(4-methylphenyl)-1H-pyrazol-1-yl]phenyl}ethanol (step 1, 0.88 mmol) in dichloromethane (10 ml) was added p-toluenesulfonyl isocyanate (221 mg, 1.06 mmol). The resulting mixture was stirred at room temperature for 30 min. The reaction mixture washed with water and the organic phase was dried (Na2SO4). After removal of the solvent, the crude product was purified by TLC with toluene/ethanol (10:1) and SCX eluting with 2 M NH3 methanol solution to afford 155 mg (35%) of the title compound as white solids: MS (ESI) m/z 545 [M+H]+, 543 [M−H]−, 1H-NMR [DMSO-d6 (dimethyl-d6 sulfoxide)]δ 7.48 (2H, d, J=8.1 Hz), 7.32-7.20 (4H, m), 7.27-7.10 (4H, m), 7.07-7.04 (2H, d, J=8.1 Hz), 3.80 (2H, t, J=6.8 Hz), 2.69 (2H, t, J=6.8 Hz), 2.23 (3H, s), 2.19 (3H, s), 2.14 (3H, s), 2.09 (3H, s).

1. washThe reaction mixture washed with water
2. dry with materialthe organic phase was dried (Na2SO4)
3. customAfter removal of the solvent
4. customthe crude product was purified by TLC with toluene/ethanol (10:1) and SCX
5. washeluting with 2 M NH3 methanol solution