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ChemicalBook CAS DataBase List 3,3-Dimethyl-2-oxobutyric acid
815-17-8

3,3-Dimethyl-2-oxobutyric acid synthesis

10synthesis methods
-

Yield:815-17-8 200 kg

Reaction Conditions:

Stage #1:1,1-dichloro-3,3-dimethylbutan-2-one with sodium hydroxide in water for 3 h;Large scale;
Stage #2: with potassium permanganate in water at 55; for 8 h;Large scale;Temperature;

Steps:

2 Example 2
1) Hydrolysis reaction: To a 2000 L enamel reactor, 300 kg of dichloro-pyridone and 300 kg of water were added,Stirring warming,Heating to 70 after the insulation,5h dropping 1000kg concentration of 30% of the liquid base,Liquid base added to continue after the reaction 3h,Obtaining an aqueous solution containing the intermediate for use;2) Oxidation reaction: 250 kg of potassium permanganate was added to the aqueous intermediate solution obtained in step 1) in five portions,Each batch plus 50kg, during the temperature control 55 ,5h, after adding potassium permanganate, continue to react after 3h to end the reaction,Filtration, collecting filtrate,The filtrate was adjusted to pH = 1 with concentrated hydrochloric acid,After adjusting the pH,The filtrate was extracted with 500 kg of dichloromethane to obtain an organic layer,The organic layer was distilled at atmospheric pressure to 100 ° C,And then cooled to 40 ,Slowly add 300kg petroleum ether temperature 8 stirring reaction 5h,Centrifugal reaction liquid,The product 200kg.

References:

Huzhou Hengyuan Biochem. Tech. Co., Ltd.;Ma, Weiheng CN105884606, 2016, A Location in patent:Paragraph 0024; 0025; 0026; 0027

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