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ChemicalBook CAS DataBase List CYCLOPENTYL PHENYL KETONE
5422-88-8

CYCLOPENTYL PHENYL KETONE synthesis

9synthesis methods
In 100ml round-bottomed flask, by 2-cyclopenta ethyl benzoylacetate (10.6g, 43.05mmol, 1.0eq), NaOH (2.6g, 64.5mmol) and Na2CO3(4.5g, 43mmol), is suspended in 50.0mLH2In O, it is warmed up to 80 DEG C and reacts 3 hours, obtain product phenylcyclopentyl ketone.Purify: reactant liquor is cooled to room temperature, extract 3 times with ethyl acetate 20mL;Organic phase saturated sodium-chloride washs, and merges organic phase and uses anhydrous MgSO4Being dried, then remove solvent under reduced pressure, obtain thick product, column chromatography purifies, and eluant, eluent is ethyl acetate: petroleum ether (1:10), obtains 6.54g target product, yield 87.2%.
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Yield:5422-88-8 62%

Reaction Conditions:

with dipotassium peroxodisulfate;iron(III)-acetylacetonate;di-tert-butyl peroxide in ethyl acetate at 120; for 12 h;

Steps:

6 Example 6

The benzoyl formic acid (30.0mg, 0.2mmol), Fe(acac)3 (21.2mg, 0.06mmol),Cyclopentyl formaldehyde (98.0mg, 1.0mmol), DTBP (58.5mg, 0.4mmol),K2S2O8 (81.1mg, 0.3mmol) and a stirring rod were put into the reaction tube, and ethyl acetate 1mL was added as a solventClose the reaction tube. Place the reaction tube in an oil bath at 120 ° C, start stirring, and perform constant temperature reaction for 12 hours.After cooling the reaction mixture to room temperature, the solid residue was filtered through a short silica gel column and washed with 10 mL of ethyl acetate.After evaporating the solvent in vacuo, the crude product was subjected to column chromatography with petroleum ether: ethyl acetate = 70: 1 as the eluent to obtain a pure product.Colorless oil, 62% yield.

References:

CN111056890,2020,A Location in patent:Paragraph 0039-0040

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