奥卡西平及其中间体的新合成方法  

A New Synthesis Method of Oxcarbanzepine and Its Intermediate

作　　者：张胜建[1] 应丽艳[1] 江海亮[1] 张洪[1] 

机构地区：[1]浙江大学宁波理工学院,浙江宁波315100

出　　处：《精细化工》2008年第12期1236-1239,共4页Fine Chemicals

摘　　要：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 synthesis method of oxcarbanzepine （OCBZ） and its intermediate was introduced in this paper. 5H-Dibenz [ b, f] azepine-5-formyl chloride was used as the starting material, via bromination,ammonolysis and hydrolysis to give OCBZ with the total yield about 62% and purity over 99. 0%. The optimum conditions for ammonolysis process were n（ NH3 ）/n（ 10,11-dibromo-5H-dibenz [ b, f] azepine-5-formyl chloride） = 5, temperature about 20℃ and time about 35 h. The yield of 10- bromo-5H-dibenz[ b,f] azepine-5-formamide is 〉 98% and its purity 〉 98. 0%. At high temperature in the ammonolysis process, 10, ll-dibromo-5H-dibenz [b, f] azepine is easy to form as a main byproduct. Structures of main products and byproducts were identified by elementary analysis and MS. The novelty of this work has been verified by Novelty Search Innovation Report of Science and Technology （Report No. 200833B210143 ） of Institute of Scientific and Technical Information of Zhejiang on Jan. 8,2008. The process has been tested in 1 t/a pilot plant and the result showed that the average yield is about 61% ,and molar fraction of the product is over 99. 1%.

关 键 词：奥卡西平 卡马西平 5H-二苯并[b f]氮杂卓-5-甲酰氯 氨解 精细化工中间体 

分 类 号：R971.6[医药卫生—药品]