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介绍了一种新的合成奥卡西平(OCBZ)及其中间体的方法:以5H-二苯并[b,f]氮杂卓-5-甲酰氯为原料,通过加成溴化、氨解、水解得到OCBZ,总收率可达62左右,OCBZ的摩尔分数大于99.0。考察了影响氨解反应的因素,优化条件为n(NH3)/n(10,11-二溴-5H-二苯并[b,f]氮杂卓-5-甲酰氯)=5,反应温度约20℃,反应时间约35h,10-溴-5H-二苯并[b,f]氮杂卓-5-甲酰胺收率大于98,摩尔分数大于98.0。结果表明,温度高时氨解反应主要易生成副产物10,11-二溴-5H-二苯并[b,f]氮杂卓。主要产物及副产物的结构均用元素分析和MS进行了确证。该文报道工作的新颖性,已为浙江省科技信息研究院2008年1月8日出具的第200833B210143号《科技查新报告》所证实。该工作已进行1t/a规模的中试,结果为:平均收率约61,产品摩尔分数大于99.1。
A new method for synthesizing oxcarbazepine (OCBZ) and its intermediates is introduced. The method is as follows: starting from 5H-dibenzo [b, f] azepine-5-carbonyl chloride, , The hydrolysis of OCBZ, the total yield of up to about 62, OCBZ mole fraction greater than 99.0. The factors influencing the aminolysis reaction were investigated. The optimum conditions were n (NH3) / n (10,11-dibromo-5H-dibenzo [b, f] azepine- About 20 ℃, the reaction time is about 35h, the yield of 10-bromo-5H-dibenzo [b, f] azepine-5-carboxamide is more than 98 and the mole fraction is more than 98.0. The results showed that at high temperature, the aminolysis reaction is mainly easy to generate by-product 10,11-dibromo-5H-dibenz [b, f] azepine. The structures of the main products and by-products were confirmed by elemental analysis and MS. This article reports the novelty of the work and has been confirmed by the Science and Technology Examination Report No. 200833B210143 issued by Zhejiang Science and Technology Information Institute on January 8, The work has been carried out 1t / a pilot scale, the result is: the average yield of about 61, the product mole fraction greater than 99.1.