Preparation method of prohexadione calcium
A technology of prohexadione and dioxocyclohexanecarboxylate, which is applied in the field of preparation of prohexadione calcium
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Embodiment 1
[0039] Place dioctyl maleate (680.00 g, 2.00 mol), acetone (84.00 g, 4.00 mol) and diethylamine (14.60 g, 0.20 mol) in an autoclave and react at 150 ℃ for 24 h. The solvent was spin-dried under reduced pressure to obtain product 1: Diisooctyl acetonyl succinate. Transfer diisooctyl acetonyl succinate to a three-necked round bottom flask, add dropwise the ethanol solution of sodium ethoxide (1 mol / L, 2.00 mol) with mechanical stirring and control the reaction temperature below 5 ℃. After the dripping is completed, continue to stir at 5 ℃ for 2 h, then rise to room temperature and stir for 12 h; after the solution is cooled below 5 ℃, add a quantitative amount of glacial acetic acid to neutralize the reaction solution, and recover ethanol under reduced pressure to obtain the product 2:3 , 5-Dioxocyclohexanecarboxylic acid isooctyl ester. Add 1,2-dichloroethane (2.7 L) into the reaction vessel containing isooctyl 3,5-dioxocyclohexane carboxylate, and add propionyl chloride (202...
Embodiment 2
[0041] Place dioctyl maleate (680.00 g, 2.00 mol), acetone (84.00 g, 4.00 mol) and diethylamine (14.60 g, 0.20 mol) in an autoclave and react at 150 ℃ for 24 h. The solvent was spin-dried under reduced pressure to obtain product 1: Diisooctyl acetonyl succinate. Transfer diisooctyl acetonyl succinate to a three-necked round bottom flask, add dropwise the ethanol solution of sodium ethoxide (1 mol / L, 2.00 mol) with mechanical stirring and control the reaction temperature below 5 ℃. After the addition is complete, continue to stir at 5 ℃ for 2 h, then warm to room temperature and stir for 12 h; after the solution is cooled below 5 ℃, add a quantitative amount of methanesulfonic acid to neutralize the reaction solution, and recover ethanol under reduced pressure to obtain product 2 :3,5-Dioxocyclohexanecarboxylic acid isooctyl ester. Add 1,2-dichloroethane (2.7 L) into the reaction vessel containing isooctyl 3,5-dioxocyclohexane carboxylate, and add propionyl chloride (202.40 g...
Embodiment 3
[0043] Place dioctyl maleate (680.00 g, 2.00 mol), acetone (84.00 g, 4.00 mol) and diethylamine (14.60 g, 0.20 mol) in an autoclave and react at 150 ℃ for 24 h. The solvent was spin-dried under reduced pressure to obtain product 1: Diisooctyl acetonyl succinate. Transfer diisooctyl acetonyl succinate to a three-necked round bottom flask, add dropwise the ethanol solution of sodium ethoxide (1 mol / L, 2.00 mol) with mechanical stirring and control the reaction temperature below 5 ℃. After the dripping is completed, continue to stir at 5 ℃ for 2 h, then warm to room temperature and stir for 12 h; after the solution is cooled below 5 ℃, add a quantitative amount of phosphoric acid to neutralize the reaction solution, and recover ethanol under reduced pressure to obtain the product 2:3, Isooctyl 5-dioxocyclohexane carboxylate. Add 1,2-dichloroethane (2.7 L) into the reaction vessel containing isooctyl 3,5-dioxocyclohexane carboxylate, and add propionyl chloride (202.40 g, 2.20 mo...
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