| 摘要 |
Astemizole drug intermediates N-(4-fluorobenzyl) phthalimide synthesis method, comprising the following steps: equipped with a stirrer, a thermometer, a reflux condenser and a dropping funnel, the reaction vessel was added 0.21 mol stannous chloride, 230ml nitromethane, 0.51mol N-aminomethyl phthalimide (2), controlling the stirring speed 130-170rpm, raised the solution temperature to 60-65 0C, held at reflux for 3-4h, added 0.71-0.73mol fluorobenzene (3), after the temperature was raised to 70-75 0C, continued reactions for 19-21 h, reducing the solution temperature to 10-15 0C , 230ml potassium chloride solution was added, added 90ml oxalic acid solution, holding stirring speed 140-160rpm, maintaining 90-120min, the precipitated solid was suction filtered, washed with salt solution, dehydrated with dehydrating agent, washed with cyclohexane solution , recrystallized from acetonitrile solution, got white crystals N-(4-fluorobenzyl) phthalimide . |
