反应详情

A solution of 5.7 g of (5-bromomethylisoxazol-3-yl)-4-fluorophenylmethanone in 100 ml of Et2O was added to a solution of 6.5 g of N-beta-hydroxyethylpiperazine in 400 ml of 25% acetone/Et2O. The resulting mixture was stirred at room temperature for 24 hours. This mixture was filtered and the solution was concentrated in vacuo to give an oil. The residue was dissolved in 300 ml of H2O and shortly thereafter a precipitate formed. The solid was filtered and dried to give 5.2 g of crude solid. A solution of 4.3 g of the amine in 50 ml of 50% ethyl acetate/CH2Cl2 was added dropwise to a solution of excess maleic acid in 600 ml of Et2O. The precipitated salt was filtered and recrystallized from 160 ml of isopropanol to yield 5.2 g (55%) of crystals, m.p. 139°-140°.

1. filtrationThis mixture was filtered
2. concentrationthe solution was concentrated in vacuo
3. customto give an oil
4. customshortly thereafter a precipitate formed
5. filtrationThe solid was filtered
6. customdried
7. customto give 5.2 g of crude solid
8. filtrationThe precipitated salt was filtered
9. customrecrystallized from 160 ml of isopropanol