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CAS No. : | 37830-90-3 | MDL No. : | MFCD00135139 |
Formula : | C5H6O3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | QYIOFABFKUOIBV-UHFFFAOYSA-N |
M.W : | 114.10 | Pubchem ID : | 142210 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80.7% | Stage #1: at 28 - 32℃; for 5 h; Autoclave; Large scale; Green chemistry Stage #2: at 38 - 42℃; Large scale; Green chemistry |
The autoclave with the agitation was filled with carbon dioxide gas,After the addition of the solid base catalyst sodium carbonate and potassium bicarbonate,5 kg of raw materials 3-hydroxy-2-butanone into the reactor,Control the reactor temperature at 30 ± 2 ,After stirring for 5 hours, 3-hydroxy-2-butanone was enolated,3-hydroxy-2-butanone for enolysis,The feed quality ratio is:3-hydroxy-2-butanone: sodium carbonate: potassium bicarbonate = 100: 0.5: 0.5.3-hydroxy-2-butanone,To the high pressure reactor supplementation of esterification catalyst potassium methoxide,Sodium ethoxide,among them,Feed quality ratio: 3-hydroxy-2-butanone: potassium methoxide: sodium ethoxide = 100: 0.5: 0.5.Closed reactor,So that sodium methoxide,The sodium ethoxide composition is evenly distributed in a high pressure reactor,And then bubbling carbon dioxide gas from the reaction liquid level,To the kettle pressure to 3.5MPa,The reaction temperature was controlled at 40 ± 2 ° C.During the insulation process,When the reaction is carried out for a period of time,The pressure inside the reactor is reduced,When the pressure inside the kettle is no longer reduced,Supplemented with carbon dioxide to 3.5MPa,And then adjust the temperature again to 40 ± 2 to continue the esterification reaction,Repeat the above operation,Until the temperature inside the reactor after the pressure did not decline so far,The unreacted 3-hydroxy-2-butanone was recovered.Adjust the reactor temperature to room temperature,Eliminate unreacted carbon dioxide to atmospheric pressure,To the reaction vessel was added 10 L of dichloroethane,The reaction solution containing 4,5-dimethyl-1,3-dioxol-2-one was taken out,The reaction solution was washed with distilled water to remove the aqueous phase to remove the catalyst,Until the reaction solution is neutral,After drying the reaction solution with anhydrous magnesium sulfate,After drying, the desiccant is removed by filtration,The filtrate is distilled to recover dichloroethane,The residue was cooled to 0-5 ° C,The crude solid was collected by centrifugation.The crude product was recrystallized from a mass of petroleum ether as a crystallization solvent to give the product 4,5-dimethyl-1,3-dioxol-2-one as white crystals,The single crystal yield of the white crystal was 48.23percentPurity 99.7percentTotal 3133.4g.In the same manner as in Example 13, prior to the addition of dichloroethane to the autoclave,The unreacted 3-hydroxy-2-butanone was recovered in the reaction solution,And re-as a raw material,And supplemented with fresh 3-hydroxy-2-butanone starting material to 5 kg,The rest is operated as in Example 13,The above-mentioned operation was repeated by recovering the recovered 3-hydroxy-2-butanone as a starting material,Continuous batch preparation,A total of 5248.2 g of white crystals of product 4,5-dimethyl-1,3-dioxol-2-one were obtained,The total yield reached 80.7percentPurity of 99.6percent. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
450 g | at 15℃; for 5.5 h; | Add 500 g of acetoin to the three bottle with stirring.1000gN,N-dimethylaniline, 3250g dichloroethane,Then add 1000 g of methyl chloroformate uniformly.The reaction temperature is controlled at 15°C and the reaction time is 5.5h. After completion of the reaction solution stripped to give DMDO 450g; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
850 g | at 12℃; for 6 h; | 1000 g acetoin was added to the reactor while stirring.2000gN,N-dimethylaniline,4000g dichloromethane,Then, 1500 g of ethyl chloroformate was added dropwise.The reaction temperature is controlled at 12°C and the reaction time is 6h.After the reaction was completed, DMDO 850g was desolvated; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
190 g | at 20℃; for 0.5 h; | Add 200 g of acetoin to the three-mouth bottle while stirring.600gN,N-dimethylaniline,2000g dichloromethane,Then 600 g of propyl chloroformate is added dropwise,The reaction temperature is controlled at 20°C and the reaction time is 0.5h.Upon completion of the reaction, DMDO 190g was desolvated; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
326 g | at 90℃; for 5.5 h; Large scale | 4725 g of dichloroethane was added to the DMDO that was stirred up.1012.5g N-chlorosuccinimideAnd 45g benzoyl peroxide,Reaction temperature 90°C, reaction time 5.5h,The crude product obtained DMDO-Cl 382.5g, a yield of 85.00percent; Step 3: Distillation: The DMDO-Cl crude product at -0.1MPa vacuum,Distilled at 110°C to produce 326g of DMDO-ClThe purity by gas chromatography was 99.06percent. |
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