BENDIOCARB synthesis

Yield:22781-23-3 91.2%

Reaction Conditions:

with triethylamine in 5,5-dimethyl-1,3-cyclohexadiene at 60; for 2 h;Temperature;Solvent;

Steps:

1-5
To the solution of the intermediate 2,2-dimethyl-4-hydroxy-1,3-benzodioxan in xylene, 0.5 g of triethylamine was added.43 g (0.75 mol) of methyl isocyanate was added dropwise at 60 ° C, and the mixture was dripped in 10 minutes.After the addition was completed, the reaction was kept at 60 ° C for 2 h.Liquid phase detection of 2,2-dimethyl-4-hydroxy-1,3-benzodioxan when the unconverted ratio is less than 1.2% by weight, the insulation is stopped.Cool down to 15-20 ° C, filter the insects and wet products,Drying at 50 ° C under vacuum to obtain the insecticide dry powder,It is a white powder. The mother liquor is concentrated and crystallized several times and filtered.The collected trivialin was recrystallized from toluene.Get the evil insects boutique.The insecticide has a yield of 91.2% based on 2,2-dimethyl-4-hydroxy-1,3-benzodioxan and a purity of more than 95%.The entire inferior preparation process takes 6-7 hours.

References:

Shandong Weifang Runfeng Chemical Co., Ltd.;Sun Guoqing;Hou Yongsheng;Xu Gaofei;Li Haihua;Li Hongli CN110054609, 2019, A Location in patent:Paragraph 0021-0030

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