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CAS No. : | 98-78-2 | MDL No. : | MFCD01320173 |
Formula : | C6H8O3 | Boiling Point : | No data available |
Linear Structure Formula : | C5H7(O)COOH | InChI Key : | RDSNBKRWKBMPOP-UHFFFAOYSA-N |
M.W : | 128.13 | Pubchem ID : | 227798 |
Synonyms : |
|
Chemical Name : | 3-Oxo-cyclopentane-carboxylic acid |
Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P301+P312-P302+P352-P304+P340-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | 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 |
---|---|---|
96% | With thionyl chloride; at 15 - 20℃; | General procedure: To a solution of 3-oxocyclohexane carboxylic acid (63.0g, 0.443mol) in ethanol (950mL), SOCl2 (38.8mL, 0.532mol) was added at 15C. The reaction mixture was stirred at rt overnight, and then evaporated under reduced pressure. The residue was dissolved in CHCl3 (500mL) and stirred with saturated aq NaHCO3 (200mL) for 30min. The layers were separated, and the aqueous layer was extracted with CHCl3 (2×50mL). The combined organic phases were dried over Na2SO4 and evaporated in vacuo. The residue was distilled under reduced pressure to give 23. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
71% | With caesium carbonate; In N,N-dimethyl-formamide; at 20℃; for 18h; | A solution of cyclopentanone-3-carboxylic acid (5.00 g, 39 mmol), caesium carbonate (12.82 g, 39 mmol) and ethyl iodide (9.12 g, 4.75 ml, 58.5 mmol) in DMF (50 ml) was stirred at RT for 18 h. The mixture was then concentrated i. vac., the residue was taken up in toluene, the mixture was concentrated again and 2 N hydrochloric acid and EtOAc were then added. The aq. phase was extracted with EtOAc (3×30 ml) and the combined organic phases were washed with aq. sodium thiosulfate soln. The organic phase was dried with Na2SO4 and concentrated i. vac.Yield: 4.34 g (71%) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
33% | With ammonium peroxydisulfate; silver nitrate; In water; acetonitrile; at 60℃; for 2h; | General procedure: Toa vial was added pyrimidine (0.42-0.65 mmol, 1.0 equiv.) (if solid), carboxylic acid (3.0 equiv.) (if solid), silver nitrate (4.0 equiv.) and ammonium persulfate (5.0equiv.). Acetonitrile (5 mL) and water(5 mL) were then added (followed by the pyrimidine and/or carboxylic acid if liquids) and the vial was capped and heated to 60 C for 2 h. The reaction mixture was monitored by TLC and LCMS. The reaction mixture was quenched by the addition of concentrated ammonium hydroxide (0.8 mL) and water (3.2 mL), diluted with brine and filtered through Celite. The filtrate was then extracted with DCM (3 x10 mL) and the organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo. The residue was adsorbed onto silica and purified by flash chromatography (0-50% EtOAc in heptane) to afford the desired compound. |
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