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ChemicalBook CAS DataBase List 1,3-Cyclopentanedione
3859-41-4

1,3-Cyclopentanedione synthesis

11synthesis methods
-

Yield:591-12-8 28% ,591-11-7 8% ,3859-41-4 17% ,108-29-2 47%

Reaction Conditions:

with bis(η5-cyclopentadienyl) titanium dichloride;potassium-t-butoxide;hydrogen;isopropylmagnesium chloride lithium chloride in tetrahydrofuran at 100; under 5171.62 Torr; for 24 h;Schlenk technique;Glovebox;Autoclave;

Steps:

4.2. General procedure for the hydrogenation of levulinic acid with[Cp2TiCl2]

General procedure: Inside a glovebox [Cp2TiCl2] (3.1 mg, 0.0124 mmol) was dissolvedin 1.5 ml of THF in the vase of a 22 ml stainless steel autoclave(4703 series, Parr Instrument Co), then 0.019 lL of a 2 Msolution of iPrMgCl in THF was added (the color of the solutionchanges to gray - green), the solution was left stirring for 5 minafter which tBuOK (116.4 mg, 1.0376 mmol) was added to the mixture.LA was then dissolved in 1.5 ml of tBuOH was added. Finally,the autoclave was pressurized with 100 psi H2 (Praxair, 99.9999 %)and heated in an oil bath at 100 C for 24 h. After the reaction time,H2 was released from the autoclave to the fume hood at room temperature. The reaction mixture was treated with an aqueous solutionof 10 % HCl to pH 7 and then extracted with ethyl acetateand analyzed by GC-MS.

References:

Roa, Diego A.;Garcia, Juventino J. [Journal of Catalysis,2022,vol. 413,p. 1028 - 1033]

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