|
|
|
| Optimization of synthesis process of chloroacetyl catechol by RSM |
| Chen Xiaoyang1, Gao Qingwei1, Ma Yaling2, Sun Yaoran1, Li Jingmeng1 |
| 1. School of Chemical Engineering, Shijiazhuang University, Shijiazhuang 050035, China; 2. Quality Assurance, Shijiazhuang Yiling pharmaceutical Corporation Ltd., Shijiazhuang 050035, China |
|
|
|
|
Abstract Carbazochrome is one of the conventional hemostatic drugs with superior therapeutic ability, so there is a huge market demand in China and even in the world. The RSM(response surface method)in Design Expert software was used to optimize the synthesis conditions of chloracetyl catechol. The Box-Behnken design experiment was used to optimize the effects of raw material molar ratio(catechol∶ chloroacetyl chloride), reaction temperature and reaction time on the synthesis yield, and the obvious influencing factors were analyzed. The best synthesis conditions were optimized by the interaction between the properties and influencing factors. Finally, the product was characterized. The optimal process conditions are as follows: the molar ratio of catechol to chloroacetyl chloride is 0.9, the reaction temperature is 44.05 ℃, the reaction time is 4.23 h, and the product yield is 75.606 8%. According to the optimized process, the yield of the actual synthesized products is 75.03%, which is close to the predicted result.
|
|
|
|
|
|
| [ 1 ] 王金玺,包振伟,刘 笑,等. 响应曲面法优化平菇多糖提
取工艺[ J ]. 中国酿造,2013,32( 4 ):108 - 112.
[ 2 ] 黄倩秋,王育琴,史录文. 卡巴克络注射剂致过敏反应[ J ]. 药物不良反应杂志,2007( 3 ):189 - 224.
[ 3 ] 王 征,孙其荣,钟延强. 卡巴克络止血气雾膜剂的制备研究王征[ J ]. 第二军医大学学报,2000,21( 10 ):975 - 976.
[ 4 ] 李 娜,张 彦,陈 萍. Box-Behnken响应曲面法优化盐炙杜仲炮制工艺的研究[ J ]. 化工科技,2018,26( 1 ):32 - 35.
[ 5 ] 段 晶,王文浩,周集义,等. Friedel-Crafts反应催化剂的研究进展[ J ]. 化学推进剂与高分子材料,2009,7( 5 ):15 - 28.
[ 6 ] 申利英,高玉红,任立伟,等. 响应曲面法优化金花葵总黄酮超声提取工艺[ J ]. 煤炭与化工,2017,40( 9 ):24 - 31.
[ 7 ] 徐丽萍,吴媛媛,王 鑫,等. 响应曲面法优化红树莓多糖提取工艺[ J ]. 中国食品添加剂,2017( 9 ):182 - 187.
[ 8 ] 杨玉娜. 响应曲面法优化β-环糊精微球固化香精工艺的研究[ D ]. 陕西科技大学,2013.
[ 9 ] 于宏伟,郧海丽,姚清国,等. 硬脂酸亚甲基面外弯曲振动变温FT-IR光谱研[ J ]. 红外技术,2013,35( 7 ): 448 - 452.
[ 10 ] 高鸿宾. 有机化学(第四版)[ M ]. 北京:高等教育出版社,2005:297 - 301. |
|
|
|