Intermediate used for synthesizing benzothiadiazole malononitrile, its synthesis method and method for detecting cn-
A technology of benzothiadiazole malononitrile and synthesis method, which is applied in the field of CN-detection, and can solve the problems of rapid poisoning and the like
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[0047] 1. be used for the intermediate of synthetic benzothiadiazole malononitrile, as shown in formula (Ⅲ):
[0048]
[0049] 2. For the synthesis of the intermediate of benzothiadiazole malononitrile and the synthetic method of benzothiadiazole malononitrile, the synthetic route is as follows figure 1 shown, including the following steps:
[0050] (1) Synthesis of intermediate TPA-BTD-Br;
[0051] Place 2.7568g of 4-dianilinophenylboronic acid, 2.3576g of 4,7-dibromo-2,1,3-benzothiadiazole, 0.1342g of 4-(triphenylphosphine) palladium and 1.7880g of potassium carbonate In a 250mL three-neck flask, add 60mL tetrahydrofuran THF, 45mL toluene and 22mL distilled H2O to the mixture. 2 O, then add 0.1mL methyl trioctyl ammonium chloride dropwise; add a magnet and stir fully, reflux reaction under nitrogen atmosphere for 16h, the temperature of reflux reaction is 85°C; after the reaction, add 200mL distilled water to the reactant, and then Extract the organic phase with dichlo...
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