反应详情

A solution of 3.7 g of (5-bromomethylisoxazol-3-yl)-4-fluorophenylmethanone in 100 ml of Et2O was added dropwise to a solution of 5.2 g of N-phenylpiperazine in 400 ml of 20% acetone/Et2O. The resulting mixture was stirred at room temperature for 24 hours. This mixture was filtered and the solution was washed with water (2×200 ml) and saturated NaCl, and dried over MgSO4. Concentration of the product gave 5.5 g of a solid which was dissolved in 100 ml of CH2Cl2 and stirred with 5 g of SiO2. This mixture was filtered, the silica washed with CH2Cl2, and the organics were evaporated to give 3.7 g of a solid. The amine was recrystallized from 135 ml of 8% toluene/hexane to yield 2.5 g (53%) of needles, m.p. 94°-95°.

1. filtrationThis mixture was filtered
2. washthe solution was washed with water (2×200 ml) and saturated NaCl
3. dry with materialdried over MgSO4