Preparation method of flumioxazin
A technology of flumechlor propargyl and difluoronitrobenzene, which is applied in the field of preparation of flumechlor propargyl, can solve the problems of high cost, low purity, and many by-products of flumecil propargyl, and achieve environmental pollution Small size, low cost of raw materials, and less by-products
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[0015] Specific embodiment 1: This embodiment is a preparation method of flumioxazin, which is specifically carried out according to the following steps:
[0016] 1. Synthesis of 2-(5-fluoro-2-nitrophenoxy) methyl acetate: Add 2,4-difluoronitrobenzene, sodium metal and THF together into a four-necked flask, under stirring conditions Add methyl glycolate dropwise, then warm up from room temperature to 65°C, reflux and stir at 65°C for 5h, evaporate the solvent to obtain solid I, wash solid I with water, and then recrystallize with ethanol as a solvent to obtain 2-(5-fluoro -2-nitrophenoxy) methyl acetate; the volume ratio of the amount of the 2,4-difluoronitrobenzene substance to the THF is 1 mol: (1.3L~1.7L); the 2, The ratio of the amount of 4-difluoronitrobenzene and sodium metal is 1:(1.8~2); the ratio of the amount of 2,4-difluoronitrobenzene to methyl glycolate is 1 :(1.8~2);
[0017] 2. Synthesis of 7-fluoro-2H-1,4-benzoxazine-3(4H)-one: add iron powder to glacial acetic ac...
Example Embodiment
[0023] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the solvent is evaporated in step 1 using a rotary evaporator. Others are the same as the first embodiment.
Example Embodiment
[0024] Specific embodiment three: This embodiment is different from one of specific embodiments one or two in: the 6-nitro-7-fluoro-2H-1,4-benzoxazine-3 (4H) described in step four ) The volume ratio of the amount of ketone to THF is 1 mol:5.5L. Others are the same as the first or second embodiment.
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