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CAS No. : | 1501-05-9 | MDL No. : | MFCD00004411 |
Formula : | C11H12O3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | SHKWSBAVRQZYLE-UHFFFAOYSA-N |
M.W : | 192.21 | Pubchem ID : | 73914 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | 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 |
---|---|---|
Triethylamine (1.4 mL, 10 mmol) was added to a stirred suspension of [delta]-oxobenzenepentanoic acid (1.92 g, 10 mmol) and (4-methylphenyl)hydrazine hydrochloride (1.59 g, 10 mmol) in ethanol (16 mL) and the mixture was stirred at room temperature for 4 h. Ether (100 mL) was added, the mixture was filtered and the solvent was evaporated under reduced pressure. The residue was added slowly to trifluoroacetic acid (15 mL) and the mixture was heated under reflux for 2 h. The mixture was cooled, water (100 mL) was added and the mixture was extracted with ethyl acetate (100 mL). The organic fraction was washed with brine (30 mL), dried (MgSO4) and the volume was reduced to Ca. 10 mL by evaporation under reduced pressure. The precipitate was collected and recrystallized from ether to give the title compound as a pale solid (1.51 g, 54percent). H NMR (360 MHz, DMSO-d6) [delta]2.39 (3H, s), 2.50-2.58 (2H, m), 3.03-3.09 (2H, m), 6.91-6.95 (1H, m), 7.23-7.25 (1H, m), 7.34-7.40 (2H, m), 7.47-7.63 (4H, m), 11.4 (1H, br s), and 12.25 (1H, br s). m/z (ES) 280 (M+1); Prepared from [delta]-oxobenzenepentanoic acid and <strong>[60481-51-8](3,4-dimethylphenyl)hydrazine hydrochloride</strong> according to the method of Description 7 as a 2:1 mixture of isomers. H NMR (360 MHz, CDCl3) (Contains 29percent [delta]-oxobenzenepentanoic acid); 5,6-dimethyl-2-phenyl-1H-indole-3-propanoic acid (Major Isomer) [delta]7.85 (1H, s), 7.58-7.33 (5H, m), 7.37 (1H, s), 7.16 (1H, s), 3.25-3.20 (2H, m), 2.75-2.67 (2H, m), and 2.38 (6H, s); 4,5-dimethyl-2-phenyl-1H-indole-3-propanoic acid (Minor Isomer) [delta]7.92 (1H, s), 7.58-7.33 (5H, m), 7.12 (1H, t, J 8.2 Hz), 7.02 (1H, t, J 8.2 Hz), 3.35-3.31 (2H, m), 2.75-2.67 (2H, m), 2.64 (3H, s), and 2.39 (3H, s). |
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