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CAS No. : | 3128-06-1 | MDL No. : | MFCD00004412 |
Formula : | C6H10O3 | Boiling Point : | No data available |
Linear Structure Formula : | CH3COC3H6COOH | InChI Key : | MGTZCLMLSSAXLD-UHFFFAOYSA-N |
M.W : | 130.14 | Pubchem ID : | 18407 |
Synonyms : |
|
Chemical Name : | 4-Acetylbutyric acid |
Signal Word: | Warning | Class: | |
Precautionary Statements: | P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
92%Chromat. | In water; at 160℃; for 4h;Sealed tube; | 2 mmol of acetylbutyric acid, 10 mmol of formamide and 40 mmol of water were placed in a 15 mL polytetrafluoroethylene-lined stainless steel reaction vessel.The sealed reaction kettle is placed in an oil bath that has been heated to a predetermined temperature (160 C). The reaction was carried out at 500 r/min for 240 min. The reaction vessel was taken out and cooled to room temperature with tap water. Add 13 mL of methanol to the reaction kettle.The yield of 6-methyl-2-piperidone was determined by GC,The conversion of acetylbutyrate was measured by HPLC. Using naphthalene as an internal standard to make a standard curve, The yield of 6-methyl-2-piperidone (m/z: 113.1) in the reaction mixture was determined by gas chromatography to be 92%. The conversion of acetobutyrate was determined by liquid chromatography to be 100%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66% | In ethanol; water; at 100℃; for 16h; | General procedure: The binucleophile (1eq.) and the ketoacid (1 eq.) are dissolved in water at the concentration of 0.125 M. If necessary, ethanol might be added to solubilise reagents (up to water/ethanol 2/1). The mixture is heated at 100 C for 16 h until complete evaporation of solvents. After completion of the reaction, the crude product is dissolved in AcOEt. The organic layer is washed with 1N HCl and NaHCO3 sat., and dried over MgSO4. Solvent is removed under reduced pressure. |
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