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3-hydroxy-3,5-dimethyl-hexan-2-one synthesis

3synthesis methods
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Yield:6321-14-8 98 %Spectr. ,2510-33-0 94 %Spectr.

Reaction Conditions:

with silver nitrate;1-ethyl-3-methylimidazolium acetate at 60; under 750.075 Torr; for 24 h;Schlenk technique;

Steps:

2.3. General procedures for the synthesis of 2-oxazolidinones and ahydroxylketones

General procedure: The synthesis of 2-oxazolidinones and a-hydroxyl ketones wasperformed in a 15 mL Schlenk tube. AgNO3 (0.0125 mmol,0.25 mol%), [C2C1im][OAc] (6 mmol), 2-aminoethanols (5 mmol)and propargyl alcohols (7.5 mmol) were first added. Then the systemwas purged with CO2 three times and the mixture was stirredat 60 °C under 0.1 MPa of CO2 for 12 h. Afterwards, the mixture wasextracted with diethyl ether (5 x 10 mL) and the upper layers werecollected and concentrated under vacuum to give the raw products,which were further purified by column chromatography on silicagel using petroleum ether/ethyl acetate (v/v, 5:1-1:1) as the eluent.When the recyclability of the catalytic system was investigated, thelower layer was recycled and reused directly for the next roundafter drying under vacuum at 60 °C for 4 h.

References:

Bu, Chao;Chaemchuen, Somboon;Chen, Cheng;Du, Minchen;Gong, Yanyan;Hu, Jia;Verpoort, Francis;Yuan, Ye;Zhang, Yongxing [Journal of Catalysis,2021,vol. 393,p. 70 - 82]