Epoxiconazole preparation method thereof
The technology of epoxiconazole and fluorobenzene is applied in the field of preparation and preparation of epoxiconazole, which can solve the problems of high environmental requirements for preparation of epoxiconazole, complicated preparation method of epoxiconazole, and failure of preparation, and achieves low cost and high cost. Stereoselective, step-by-step effects
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Embodiment 1
[0017] Embodiment one: a kind of preparation method of epoxiconazole comprises the following steps:
[0018] 1) Add fluorobenzene and solvent into a glass reaction bottle with a stirrer and a condenser. The ratio of fluorobenzene to acetyl chloride is 1:15. Considering the toxicity and cost, choose dichloroethane as the solvent, and stir Add dichloroethane dropwise, control the reaction temperature, and wait for 5 hours to fully react in the glass reaction bottle. After the reaction is completed, hydrolyze with hydrochloric acid, steam distill off excess fluorobenzene, and solvent extraction precipitates to obtain p-fluorobenzene ethyl ketone;
[0019] 2) Add o-chlorobenzyl phosphate and n-butanol solvent into a reaction flask with a stirrer and a condenser, continue heating from 0°C to 150°C, add p-fluoroacetophenone and o-chlorobenzyl phosphoric acid dropwise under stirring The ratio of ester to p-fluoroacetophenone is 1:2, and the temperature is kept at 50°C for 12 hours t...
Embodiment 2
[0024] Embodiment two: a kind of preparation method of epoxiconazole comprises the following steps:
[0025] 1) Add fluorobenzene and solvent into a glass reaction bottle with a stirrer and a condenser. The ratio of fluorobenzene to acetyl chloride is 1:15. Considering the toxicity and cost, choose dichloroethane as the solvent, and stir Add dichloroethane dropwise, control the reaction temperature, and wait for 5 hours to fully react in the glass reaction bottle. After the reaction is completed, hydrolyze with hydrochloric acid, steam distill off excess fluorobenzene, and solvent extraction precipitates to obtain p-fluorobenzene ethyl ketone;
[0026] 2) Add o-chlorobenzyl phosphate and n-butanol solvent into a reaction flask with a stirrer and a condenser, continue heating from 0°C to 150°C, add p-fluoroacetophenone and o-chlorobenzyl phosphoric acid dropwise under stirring The ratio of ester to p-fluoroacetophenone is 1:2, and the temperature is kept at 75°C for 12 hours. ...
Embodiment 3
[0031] Embodiment three: a kind of preparation method of epoxiconazole comprises the following steps:
[0032] 1) Add fluorobenzene and solvent into a glass reaction bottle with a stirrer and a condenser. The ratio of fluorobenzene to acetyl chloride is 1:15. Considering the toxicity and cost, choose dichloroethane as the solvent, and stir Add dichloroethane dropwise, control the reaction temperature, and wait for 5 hours to fully react in the glass reaction bottle. After the reaction is completed, hydrolyze with hydrochloric acid, steam distill off excess fluorobenzene, and solvent extraction precipitates to obtain p-fluorobenzene Ethyl ketone, purity 93.2%, yield 82.1%;
[0033] 2) Add o-chlorobenzyl phosphate and n-butanol solvent into a reaction flask with a stirrer and a condenser, continue heating from 0°C to 150°C, add p-fluoroacetophenone and o-chlorobenzyl phosphoric acid dropwise under stirring The ratio of ester to p-fluoroacetophenone is 1:2, and the temperature i...
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