反应详情

To a solution of 1-[3-chloromethyl-4-(methylsulfonyl)phenyl]-5-[4-(2-furyl)phenyl]-3-(trifluoromethyl)-1H-pyrazole from step1 (70 mg, 0.15 mmol) in THF (3.0 mL), methylamine (5.0 ml, 10 mmol, 2.0 M in THF) and K2CO3 (200 mg, 1.5 mmol) was added at room temperature and stirred for 1 hour. The mixture was concentrated and ethyl acetate (30 mL) was added, dried over MgSO4, and concentarted in vacuo. The solid was dissolved in 10% methanolic HCl (10 mL), and volatiles were removed by evaporation. The residual solid was recrystallized from ethanol to give the title compound (45 mg, 59%).

1. concentrationThe mixture was concentrated
2. additionethyl acetate (30 mL) was added
3. dry with materialdried over MgSO4
4. dissolutionThe solid was dissolved in 10% methanolic HCl (10 mL)
5. customvolatiles were removed by evaporation
6. customThe residual solid was recrystallized from ethanol