| 摘要 |
Glycopyrrolate pharmaceutical intermediates benzoyl nitrile synthesis method, comprising the following steps: the reaction vessel was added 1.31-1.33mol cyanamide (3), added 1.1 mol benzoyl bromide (2) , 0.3mol stannous chloride, 300ml nitromethane, controlled stirring speed at 130-160rpm, raised solution temperature to 240-245 0C, the reaction continued for 3-4 h, 230--240 0C fractions were collected in a condenser, after the cold curing, the resulting solid was washed with 500ml sodium sulfite solution for 5-6 times, washed with saline solution for 2-3 times, washed in ethylenediamine solution, partitioning, the organic layer was dehydrated with dehydrating agent, low pressure distillation, 180--185 0C fractions were collected, and cooled to solidify, got colorless crystals benzoyl nitrile . |
