摘要
在1,2-二氯乙烷中,以30%H2O2为氧化剂,过氧磷钨酸季铵盐[π-C5H5N(CH2)11CH3]3PW4O32为催化剂,催化松油烯-4-醇的氧化反应生成对孟烷-1,2,4-三醇;该产物以白色粉末状固体析出,容易通过简单过滤方法分离,其结构经元素分析、红外光谱、1H NMR及13C NMR确证。本实验最佳合成工艺条件为:松油烯-4-醇12.3 mmol,1,2-二氯乙烷5 mL,过氧化氢与松油烯-4-醇的物质的量之比1.25∶1,催化剂用量为2.98%(以松油烯-4-醇的质量分数计),温度50℃,反应时间1.5 h;在此条件下,松油烯-4-醇的转化率和对孟烷-1,2,4-三醇的产率分别达到99.8%和58.0%,纯度达到98%以上。初步除草活性测试表明,对孟烷-1,2,4-三醇对水稻稗草种子萌发后胚根与幼芽的生长具有明显的影响,在10 mmol/L的浓度下,根长抑制率和芽长抑制率分别为100%和81.4%。
Oxidation of 4-terpineol with 30% H202 catalyzed by quaternary ammonium peroxotungsto-phosphate catalyst B＇-C5 H5 N （ CH2 ） 11CH3 ] 3 PW4 032 in 1,2-dicbloroethane gave p-menthane-1,2,4-trio1. The product was easily separated as a white crystalline powder by filtration and structurally identified by means of EA, IR, 1 H NMR and 13 C NMR. Under the optimal reaction conditions, i. e. 4-terpineol 12.3 mmol, 1,2-dichloroethane 5 mL, molar ratio of hydrogen peroxide to 4-terpineol 1.25 ： 1, mass percentage of catalyst to 4-terpineol 2.98%, reaction temperature 50 ~C, reaction time 1.5 h, the conversion rate of 4-terpineol and yield of p-menthane-1,2,4-triol were 99.8% and 58.0% , respectively. The purity of product can reach more than 98%. The preliminary herbicidal assay had that p-menthane-1,2,4-triol had an obvious post-emergence inhibitory effect against shoot growth and root elongation of barnyard grass （Echinochloa crusgalli L. ）. The percentage inhibition of root growth and shoot elongation at 10 mmol/L concentration in herbicidal test were 100% and 81.4%, respectively.
出处
《生物质化学工程》
CAS
2013年第5期40-44,共5页
Biomass Chemical Engineering
基金
广西科技攻关项目(1348006-10)
广西自然科学基金(2011GXNSFA018057)
广西民族大学引进人才科研启动项目(2010QD020)
