精盖草能的合成  

Synthesis of R-(+)-Haloxyfop-methyl

作　　者：袁冠华[1] 严成武[1] 

机构地区：[1]江苏安邦电化有限公司,江苏淮安223002

出　　处：《江苏化工》2004年第4期26-28,33,共4页Jiangsu Chemical Industry

摘　　要：研究了以碳酸钾作为缚酸剂,四丁基溴化胺作为相转移催化剂,二甲亚砜为溶剂,R-(+)-2-(4-羟基-苯氧基)-丙酸甲酯和2,3-二氯-5-(三氟甲基)-吡啶发生醚化反应,得到精盖草能的方法,讨论了溶剂种类、催化剂用量、反应时间对反应产率的影响。结果表明:室温下反应37h,用水稀释,乙醚萃取,无水硫酸钠干燥,蒸馏脱去乙醚,得到精盖草能,用旋光仪检测产品的旋光度,经元素分析、IR、1HNMR证实其结构与预期结构相符。收率为88%。通过计算得到精盖草能的[α]=+24.3°,其光学纯度=76.9%,质量分数为94%。R-(+)-haloxyfop-methyl was prepared through the etherifying between R-(+)-methyl-2-(4-hydrophenoxy) propionate and 2,3-dichloro-5-trifluromethyl-pyridine. Dilute methyl R-(+)-2-(4-hydrophenoxy) propionate with DMSO was added to 2,3-dichloro-5-trifluromethyl-pyridine in which tetrabutyl-ammonium bromide used as phase transfer catalyst and powdered anhydrous potassium carbonate used as bound acid reagent with the amount account for 4 times of total mass. The mixture was reacted for 37 h at room temperature, and the organic phase was separated and resulting products dried with anhydrous sodium sulfate while Et_2O was recycled by distillation; R-(+)-haloxyfop-methyl was thus obtained and identified by use of elementary analysis, IR, ~1 H NMR, GC-MS and polarimetry. The yield was 88% with [α]_D^(25)+24.3, e.e% of 76.9 and mass content of 94%.

关 键 词：2 3-二氯-5-三氟甲基吡啶 二甲亚砜 碳酸钾 R-(+)-2-(4-羟基-苯氧基)-丙酸甲酯 精盖草能 

分 类 号：TQ457.21[化学工程—农药化工]