| 摘要 |
Benzene carboxamide pharmaceutical intermediates trans -4-N benzyloxycarbonyl-aminomethyl-cyclohexane- 1 -carboxylic acid synthesis method , comprising the following steps: equipped with a stirrer, the reaction vessel was added 0.043 mol trans-4-aminomethyl cyclohexane-1-carboxylic acid (2), 30-40ml sodium sulfite solution, the temperature of the solution is reduced to 2 -5 0C, controlling the agitation speed 130-160rpm, dropwise added 0.05-0.053mol benzyloxycarbonyl amide (3), control dropwise addition time in 90-120min, whereupon white crystals precipitated, the resulting crystals were dissolved in 300ml potassium chloride solution, added oxalic acid solution to adjust solution pH to 6-7, the temperature of the solution is reduced to 1--3 0C, white precipitate, suction filtered, washed with saline solution, dehydrated with dehydrating agent, recrystallization in solution of triethylamine, got white needle crystals trans -4-N benzyloxycarbonyl-aminomethyl-cyclohexane-1-carboxylic acid. |
