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    • 5. 发明授权
    • 고순도 메티오졸린의 공업적 제조방법
    • 高纯度甲硫唑啉的制备方法
    • KR101201203B1
    • 2012-11-15
    • KR1020120033835
    • 2012-04-02
    • 한국화학연구원주목우연구소
    • 고영관구동완우재춘류재욱구석진황기환이동국정근회전만석김성헌임종수조남규
    • C07D413/04
    • C07D413/04B01J31/0271
    • PURPOSE: An industrial method for preparing [5-{(2,6-difluorobenzyloxy)methyl}-4,5-dihydro-5-methyl-3-(3-methylthiophene-2-yl)-isoxazole](methiozolin) is provided to obtain a large amount of the methiozolin of high purity and to cultivate agricultural crops. CONSTITUTION: A method for preparing thiozolin(chemical formula 1) comprises: a step of reacting 4,5-dihydro-5-methyl-3-{(3-methylthiophene-2-yl)-isoxazole-5-yl}methanol of chemical formula 2 with 2,6-difluorobenzyl(chloride or bromide) of chemical formula 3 using an alkali metal base and a phase converting catalyst in a mixture of water and organic solvent at 50-100 Deg. C. to prepare the concentrate of an organic layer; and a step of crystallizing the concentrate in a mixture solvent of water/ethanol, water/isopropanol, or C1-C3 alcohol/n-heptane. The organic solvent is benzene, toluene, xylene, chlorobenzene, or 1,2-dichloroethane. The alkali metal base is sodium hydroxide, potassium hydroxide, or lithium hydroxide.
    • 目的:提供制备[5 - {(2,6-二氟苄氧基)甲基} -4,5-二氢-5-甲基-3-(3-甲基噻吩-2-基) - 异恶唑](甲氧基)唑的工业方法) 获得大量高纯度的甲氧唑啉并培育农作物。 构成:制备噻唑啉(化学式1)的方法包括:将化合物的4,5-二氢-5-甲基-3 - {(3-甲基噻吩-2-基) - 异恶唑-5-基}甲醇 式2与化学式3的2,6-二氟苄基(氯化物或溴化物)使用碱金属碱和相转化催化剂在水和有机溶剂的混合物中在50-100℃下反应。 C.制备有机层的浓缩物; 以及将浓缩物在水/乙醇,水/异丙醇或C 1 -C 3醇/正庚烷的混合溶剂中结晶的步骤。 有机溶剂为苯,甲苯,二甲苯,氯苯或1,2-二氯乙烷。 碱金属碱是氢氧化钠,氢氧化钾或氢氧化锂。