3,6-二氯哒嗪-4-羧酸的合成  

Synthesis of 3,6-dichloro-4-pyridazinecarboxylic acid

作　　者：姚转乐[1] 石强[1] 樊学忠[1] 王融冰[1] 

机构地区：[1]西安近代化学研究所,陕西西安710065

出　　处：《应用化工》2009年第11期1591-1593,共3页Applied Chemical Industry

摘　　要：以柠康酸酐和盐酸联氨为起始原料，经过三步反应制得3，6-二氯哒嗪4-羧酸。通过红外、核磁共振对其结构进行了确证。考察r原料用量、氧化剂种类以及用量、反应温度、反应时间等对合成3，6-二氯哒嗪4·羧酸的影响。较佳工艺条件为：合成3，6-二羟基4＋甲基哒嗪时，柠康酸酐和盐酸联氨摩尔比为1：1．12；氯代反应时，3，6-二羟基4．甲基哒嗪和三氯氧磷摩尔比为1：6。以HNO3-KClO3为氧化剂，其与3，6-二氯4-甲基哒嗪质量比为2：1，在35-40℃反应3h。总收率达到52％，纯度大于98％。Using citraconic anhydride and hydrazin dihydrochloride as base materials, through three steps 3,6-dichloro-4-pyridazinecarboxylic acid was synthesized. Its structure was analyzed and characterized by IR and 1H NMR. The effects of material, oxidant, dosage of oxidant, reaction temperature and time on the synthesis were studied. The better technology has been obtained：the mole ratio of citraconie anhydride to hydrazin dihydrochloride is 1 ： 1.12 when 3,6-dihydroxy-4-methyl pyridazine was synthesized. The mole ratio of 3,6-dihydroxy-4-methyl pyridazine to phosphorous oxychloride is 1：6 during chlorie reaction. Tak- ing nitric acid-chlorate liquor as oxidant, mass ratio of it to 3,6-dichloro-4-methyl pyridazine is 2 ： 1, reaction time is 3 h at 35 - 40 ℃. The yield of 3,6-dichloro-4-pyridazinecarboxylie acid is 52% and purity is over 98%.

关 键 词：柠康酸酐 盐酸联氨 3 6-二氯哒嗪4-羧酸 合成 

分 类 号：O626.4[理学—有机化学]