Preparation method of beta-dione compound
A compound and diketone technology, which is applied in the field of preparation of β-diketone compounds, can solve the problems of low yield and unsafety of β-diketone compounds, and achieve the effect of high yield
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[0018] The present invention provides a method for preparing a β-diketone compound represented by formula (4), wherein the method comprises: in the presence of a solvent represented by formula (3) and an alkali metal potassium alkoxide, formula (1) ) The methyl carboxylate shown in ) reacts with the ketone shown in formula (2);
[0019] CH 3 O-CO-CR 1 R 2 R 3 Formula 1);
[0020] CH 3 -CO-CR 1 R 2 R 3 Formula (2);
[0021] R 4 O-(CH 2 (CH 2 ) n O) m -R 4 Formula (3);
[0022] R 3 R 2 R 1 C-CO-CH 2 -CO-CR 1 R 2 R 3 Formula (4);
[0023] Among them, R 1 , R 2 and R 3 each independently hydrogen or C 1 -C 4 Alkyl groups, such as R 1 , R 2 and R 3 Can each independently be one of hydrogen, methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl and tert-butyl; preferably, R 1 , R 2 and R 3 each independently hydrogen or C 1 -C 2 The alkyl groups, for example, can be independently hydrogen, methyl or ethyl; more preferably, the methy...
Embodiment 1
[0039]Add 135g (1.2mol) potassium tert-butoxide (purchased from Sinopharm Group Chemical Reagent Co., Ltd., referred to as "Sinopharm", the same below) and 104.5g (1.16mol) ethylene glycol dimethyl ether ( (purchased from Sinopharm Corporation) and heated to reflux under stirring with a mechanical stirrer to raise the temperature to 20°C. Then, a liquid mixture consisting of 319g (3.6mol) methyl propionate (purchased from Japan TCI Company) and 86.5g (1.2mol) methyl ethyl ketone (purchased from Sinopharm Corporation) was added at a constant speed through the constant pressure dropping funnel, and the dropping time for 20 minutes, then stirred at 75°C for another 4.5 hours, cooled to 40°C, added 120g of ice water, and adjusted the pH to 6 with concentrated hydrochloric acid. Then filter with a suction filter bottle to remove potassium chloride, the filtrate is separated into layers, and the organic layer and the water layer are separated. Gas chromatography analysis of the org...
Embodiment 2
[0041] Add 13.6g (0.12mol) of potassium tert-butoxide (purchased from Sinopharm) and 40mL (0.28mol) of diethylene glycol dimethyl ether into a 250ml three-neck flask, heat and reflux to 60° C. under stirring with a mechanical stirrer. Then, a liquid mixture composed of 39mL (0.41mol) methyl propionate (purchased from Japan TCI Company) and 9mL (0.1mol) butanone (purchased from Sinopharm Corporation) was added at a constant speed through a constant pressure dropping funnel, and the dropping time was 40min, then stirred at 60°C for another 4.5 hours, cooled to 40°C, added 20g of ice water, and adjusted the pH to 6 with concentrated hydrochloric acid. Then filter with a suction filter bottle to remove potassium chloride, the filtrate is separated into layers, and the organic layer and the water layer are separated. The gas chromatographic analysis of the organic layer showed that the yield of 3,5-heptanedione was 64.3% (calculated as butanone).
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