A method for the dehydrogenation self-coupling of 1,3-dicarbonyl compounds catalyzed by visible light
A dicarbonyl and compound technology, applied in the field of organic catalysis, can solve the problems of cumbersome preparation work, easy occurrence of by-products, large yield loss, etc., and achieve the effects of improving energy utilization, reducing solvent polarity, and improving efficiency.
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Embodiment 1
[0039] Weigh terpyridyl ruthenium(II) chloride hexahydrate (0.006mmol, 2% equiv) and potassium persulfate (0.45mmol, 1.5equiv) into the reactor, add ethyl benzoyl acetate (0.3mmol, 1equiv) , 1,4-dioxane (0.15mmol, 0.5equiv), mixed with solvent acetonitrile / water (V / V=1mL / 1mL). Put the reaction bottle into an oil bath at 25°C, and react for 24 hours under the irradiation of a 26W LED lamp. After the reaction, separation and purification were carried out to obtain product 1 (the reaction yield was 88%).
Embodiment 2
[0041] Weigh terpyridyl ruthenium (II) chloride hexahydrate (0.006mmol, 2% equiv) and potassium persulfate (0.45mmol, 1.5equiv) into the reactor, add ethyl p-fluorobenzoyl acetate (0.3mmol, 1equiv), 1,4-dioxane (0.15mmol, 0.5equiv), with the solvent acetonitrile / water (V / V=1mL / 1mL). Put the reaction bottle into an oil bath at 25°C, and react for 24 hours under the irradiation of a 26W LED lamp. After the reaction, separation and purification were carried out to obtain the product 2 (the reaction yield was 82%).
Embodiment 3
[0043] Weigh terpyridyl ruthenium (II) chloride hexahydrate (0.006mmol, 2% equiv) and potassium persulfate (0.45mmol, 1.5equiv) into the reactor, add ethyl p-chlorobenzoyl acetate (0.3mmol, 1equiv), 1,4-dioxane (0.15mmol, 0.5equiv), with the solvent acetonitrile / water (V / V=1mL / 1mL). Put the reaction bottle into an oil bath at 25°C, and react for 24 hours under the irradiation of a 26W LED lamp. After the reaction, separation and purification were carried out to obtain the product 3 (the reaction yield was 78%).
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