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CAS No. : | 35598-05-1 | MDL No. : | MFCD06203918 |
Formula : | C10H12O3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | OGYAVWKYDVBIMW-UHFFFAOYSA-N |
M.W : | 180.20 | Pubchem ID : | 13257269 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302 | 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 |
---|---|---|
100% | With thionyl chloride; at 20℃;Reflux; | To a stirred mixture of 4-methoxy-2-methyl benzoic acid (1.0 g, 6 mmol) and methanol (50 mL) was added thionyl chloride (1.3 mL, 17.8 mmol), dropwise, at room temperature under a nitrogen atmosphere. The reaction mixture was heated at reflux for 3 h. The reaction mixture was allowed to cool at room temperature and concentrated to give a pale yellow liquid. The crude product was purified by flash chromatography over silica with hexanes:ethyl acetate (9:1) to give 1.11 g (100%) of methyl 2-methyl-4-(methyloxy)benzoate as a colorless liquid. 1H NMR (400 MHz, DMSO-J6): delta 7.81 (d, J = 9 Hz, IH), 6.86 (d, J = 3 Hz, IH), 6.83 (dd, J = 9, 3 Hz, IH), 3.78 (s, 3H), 3.75 (s, 3H), 2.49 (s, 3H). ES-LCMS m/z 181(M + H)+. |
98% | sulfuric acid; In water; for 48h;Heating / reflux; | According to J. Org. Chem. 33: 494 (1968), a mixture of 4-methoxy-2-methylbenzoic acid (20 g, 120 mmol) and [MEOH] (97 mL) containing sulfuric acid [(CONC.,] 0.6 mL) was heated under reflux 48 h. After cooling the mixture was evaporated and the residue diluted with diethyl ether and washed with a saturated sodium hydrogen carbonate solution and brine. The organic phase was then separated and dried over sodium sulphate. After evaporation the residue was distilled through a 8 cm Vigreux column to afford the title compound (21.2 g, 98%) as a colourless liquid. Bp 60 [C/1] mbar. MS: m/e = 180.3 (M+). |
94% | With sulfuric acid; In water; at 65℃; for 18h; | 4-Methoxy-2-methyl-benzoic acid methyl esterA solution of 4-Methoxy-2-methyl-benzoic acid (15 g, 90 mmol) in methanol {200 mL) was heated to 65 0C. Sulfuric acid (8.9 g, 90 mmol) was added and the mixture was stirred for 18 h at 65 C. The reaction was cooled and concentrated and the residual oil was dissolved in ethyl acetate and washed with water, brine, and absorbed onto silica to perform chromatography (10 % ethyl acetate/hexanes) to yield 4-Methoxy-2-methyl-benzoic acid methyl ester as an oil, (15.3 g, 94 %). MS: ES M+1: 181.0 (180.1). |
84% | With sulfuric acid; for 24h;Reflux; | Benzoic acid (1 equiv) was dissolved in MeOH (1.66 mL per mmol) and H2SO4 (0.07 mL per mmol). The solution was refluxed for 7-24 h before being cooled to rt and concentrated in vacuo. The resulting mixture was dissolved in EtOAc. The organics were washed with an aqueous solution of NaOH (10 %), combined, dried over MgSO4 and concentrated in vacuo to afford the desired ester. |
81% | With thionyl chloride; for 3h;Heating / reflux; | Preparation 67 4-Methoxy-2-methyl-benzoic acid methyl esterTo an ambient temperature suspension of 4-Methoxy-2-methyl-benzoic acid (1.0 g, 6.02 mmol) in MeOH (10 mL) is added thionyl chloride (1.10 mL, 15.04 mmol) dropwise. The reaction mixture is heated to reflux. After 3h, the reaction is concentrated and the residue is partitioned between EtOAc and NaHCO3. The aqueous layer is extracted with EtOAc and the combined organic layers are washed with brine, dried (MgSO4), filtered, and concentrated to yield the title compound (877 mg, 81%) 1H NMR (400 MHz, CDCl3) delta 7.95-7.91 (m, IH), 6.77-6.72 (m, 2H), 3.86 (s, 3H), 3.84 (s, 3H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
To a solution of <strong>[35598-05-1]methyl 4-methoxy-2-methylbenzoate</strong> (11.4 g, 63.3 mmol) in THF (65 mL) at 0 C, LiAlH4 (1M in ether, 76.0 mL, 75.9 mmol) was added via addition funnel over 50 min. The ice water bath was removed, and the reaction was allowed to stir at room temperature for 30 min. Upon completion, the reaction was cooled to 0 C and sodium sulfate decahydrate was added portionwise until the bubbling ceased. The reaction was then diluted with ether and filtered. The filtrate was concentrated under reduced pressure to give (4-methoxy-2- methylphenyl)methanol (8.2 g) as a clear oil. ? NMR (300MHz, CDC13): delta 7.23 (d, 1H), 6.72 (m, 2H), 4.63 (d, 2H), 3.79 (s, 3H), 2.36 (s, 3H), 1.42 (t, 1H). |
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