Manganese catalyst and application of manganese catalyst in catalyzing epoxidation of triazole alkene to prepare epoxiconazole
A technology for catalyzing triazoles and manganese catalysts, applied in the field of pesticides, can solve problems such as hidden safety hazards, unfriendly environment, increase post-processing steps, etc., and achieve the effects of reducing environmental pressure, low system cost, and simple recovery
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[0028] Example 1:
[0029] At room temperature, 7.4 mg (0.03 mmol) of manganese acetate tetrahydrate was added to a 100 mL single-necked flask, 5 mL of acetonitrile and 22.2 mg (0.18 mmol) of picolinic acid were added, and stirring was started. Under stirring, add 3.14g (10.0mmol, content 99.68%) recrystallized triazolene, 0.43g (5.0mmol) distilled 2,3-butanedione, 24.6mg sodium acetate dispersed in 15mL acetonitrile solution, continue to stir . The flask was cooled in an ice bath and 30% hydrogen peroxide was added dropwise below 2°C. 3.40g of hydrogen peroxide was added within 5.0hrs. During this period, the dropping rate should be controlled so that the temperature of the reaction solution was not higher than 5°C. After the addition of hydrogen peroxide is completed, stir for 1.0 hr under a cold bath. Remove the ice / water bath, stir at room temperature for 2.0hrs, and concentrate under reduced pressure to obtain the target epoxiconazole. The material conversion rate is 99%, ...
Example Embodiment
[0030] Example 2:
[0031] At room temperature, 7.4 mg (0.03 mmol) of manganese acetate tetrahydrate was added to a 100 mL single-necked flask, 20 mL of acetonitrile and 22.2 mg (0.18 mmol) of picolinic acid were added, and stirring was started. Under stirring, add 3.14g (10.0mmol, content 99.68%) recrystallized triazolene and 0.43g (5.0mmol) distilled 2,3-butanedione in sequence, after stirring at room temperature for 15min, add 24.6mg sodium acetate , Continue to stir. The flask was cooled in an ice bath and 30% hydrogen peroxide was added dropwise below 2°C. Add 3.40g of hydrogen peroxide within 5.0hrs, during which the dropping rate should be controlled so that the temperature of the reaction solution is not higher than 5℃. After the addition of hydrogen peroxide is completed, stir for 1.0 hr under a cold bath. Remove the ice / water bath and stir at room temperature for 2.0 hrs. The material conversion rate is 99%, and the yield of epoxiconazole is 66% (detected by HPLC). ...
Example Embodiment
[0032] Example 3: Add 6.9 mg (0.028 mmol) of manganese acetate tetrahydrate to a 100 mL single-necked flask at room temperature, add 20 mL of acetonitrile, and 20.9 mg (0.17 mmol) of picolinic acid, and start stirring. Under stirring, add 3.14g (10.0mmol, content 99.68%) recrystallized triazolene, 0.43g (5.0mmol) distilled 2,3-butanedione, and after stirring for 15min at room temperature, add 23.0mg sodium acetate, Continue to stir. The flask was cooled in an ice bath and 30% hydrogen peroxide was added dropwise below 2°C. 3.40g of hydrogen peroxide was added within 5.0hrs. During this period, the dropping rate should be controlled so that the temperature of the reaction solution was not higher than 5°C. After the addition of hydrogen peroxide is completed, stir for 1.0 hr under a cold bath. Remove the ice / water bath, stir at room temperature for 2.0hrs, and concentrate under reduced pressure to obtain the target epoxiconazole. The material conversion rate was 98%, and the yi...
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