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CAS No. : | 1461-96-7 | MDL No. : | MFCD01311172 |
Formula : | C7H10O4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | ASJCSAKCMTWGAH-SYDPRGILSA-N |
M.W : | 158.15 | Pubchem ID : | 727374 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319 | Packing Group: | N/A |
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 |
---|---|---|
63% | Stage #1: With bromine In chloroform at 0 - 20℃; Stage #2: With potassium hydroxide In water at 0℃; for 6 h; Stage #3: With hydrogenchloride In water |
Br2 (112.8 g, 705.6 mmol) was added dropwise at 0 °C to a solution of ethyl 2- oxocyclohexanecarboxylate (120 g, 705.6 mmol) in chloroform (360 ml). The resulting reaction mixture was stirred at rt overnight, then washed with NaHC03 (2x200 ml) and brine (2x100 ml). The organic layer was dried over Na2S04 and concentrated and the residue was added dropwise to an ice-cold solution of KOH (168 g, 3 mol) in water (960 ml). The reaction mixture was stirred for 6 h at 0 °C, then extracted with diethyl ether. The aqueous phase was acidified with 4.0 M HCI (pH 5) and extracted with diethyl ether. The combined organic layers were washed with brine (200 ml), dried, filtered and concentrated. The afforded yellow oil was crystallized (EtOAc/diethyl ether) which gave the title compound as a colourless crystals (70 g, 63percent). MS (ESI): 159 [M+H]+. |
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