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CAS No. : | 18179-39-0 | MDL No. : | MFCD06797864 |
Formula : | C8H7IO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | WUFUURSWOJROKY-UHFFFAOYSA-N |
M.W : | 278.04 | Pubchem ID : | 11380407 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
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* 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% | With sodium hydroxide; water; In tetrahydrofuran; methanol; at 40℃; | 40 g (1 mol) of sodium hydroxide are added to 55.6 g (0.2 mol) of methyl 4-iodosalicylate in 600 ml of THF, 10 ml of methanol and 10 ml of water. The solution is heated at 40 C. overnight. It is then evaporated. The residue is taken up in water. It is acidified to pH 1 with concentrated hydrochloric acid and extracted with ethyl acetate. The organic phase is washed several times with water, dried over magnesium sulphate and concentrated. The product is triturated in a dichloromethane-hexane mixture and then filtered. [00486] Orange-coloured powder. m=48.53 g. Y=92%. 1H NMR (CDCl3): 7.20-7.24 (1H, dd, J=6.8 Hz, J'=1.5 Hz), 7.36-7.37 (1H, d, J=1.5 Hz), 7.52-7.56 (1H, d, J=8.3 Hz), 11.29 (1H, s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
50% | With thionyl chloride; for 10h;Reflux; | Synthesis of Compound 3 10.0 g (37.8 mmol) of Compound 2 was taken in 200.0 ml dry methanol. To this 11.5 ml (151.0 mmol) of SOCl2 was added drop wise. Then the reaction mixture was refluxed for 10 h. After completion of reaction, the reaction mixture was cooled to room temperature and methanol was evaporated to dryness under vacuum to obtain 12.0 g crude product which was further purified by washing with minimum amount of methanol to obtain 5.2 g of Compound 3. Yield: 50.0% Analysis: 1H NMR (300 MHz, CDCl3): delta 10.8 (s, 1H); 7.49 (d, 1H); 7.40 (d, 1H); 7.24 (dd, 1H); 3.9 (s, 3H). MS (m/z): 277 (M+-H) |
50% | With thionyl chloride; for 10h;Reflux; | Synthesis of Compound 3 10.0 g (37.8 mmol) of Compound 2 was taken in 200.0 ml dry methanol. To this 11.5 ml (151.0 mmol) of SOCl2 was added drop wise. Then the reaction mixture was refluxed for 10 h. After completion of reaction, the reaction mixture was cooled to room temperature and methanol was evaporated to dryness under vacuum to obtain 12.0 g crude product which was further purified by washing with minimum amount of methanol to obtain 5.2 g of Compound 3. Yield: 50.0% Analysis: 1H NMR (300 MHz, CDCl3): delta 10.8 (s, 1H); 7.49 (d, 1H); 7.40 (d, 1H); 7.24 (dd, 1H); 3.9 (s, 3H). MS (m/z): 277 (M+-H) |
With thionyl chloride; for 14h;Heating / reflux; | To a solution of <strong>[16870-28-3]2-hydroxy-4-iodobenzoic acid</strong> (35.0 g) in methanol (700 mL) was added dropwise thionyl chloride (40 mL) . The mixture was refluxed for 14 hr and concentrated. The residue was chromatographed on silica gel using n-hexane/ethyl acetate as an eluent to give the title compound as crystals (34.2 g) . mp. 690C (ethyl acetate/n-hexane) . 1H-NMR (300 MHz, CDCl3) delta: 3.94 (s, 3H) , 7.23 (dd, J = 8.4,1.8 Hz, IH) , 7.40 (d, J = 1.8 Hz, IH) , 7.50 (d, J = 8.4 Hz,IH) , 10.74 (s, IH) . |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In tetrahydrofuran; methanol; diethyl ether; at 20℃; for 2.5h; | A solution of <strong>[16870-28-3]2-hydroxy-4-iodo-benzoic acid</strong> (4.0 g, 0.015 mol) in THF (25 ml) and MeOH (25 ml) is treated by the dropwise addition of (trimethylsilyl)-diazomethane (2.0M in Et2O, 15 ml) and stirred at room temperature for 2.5 hours. Volatiles are removed in vacuo and the crude residue diluted into EtOAc. The organic phase is sequentially washed with saturated aqueous NaHCO3 (3×), saturated aqueous NaCl (1×), and H2O (1×). The organic phase is dried over MgSO4, filtered, and concentrated. The crude product is purified with silica gel column chromatography (0-80% ethyl acetate in hexanes gradient) to afford <strong>[16870-28-3]2-hydroxy-4-iodo-benzoic acid</strong> methyl ester: ESMS m/z 279.0 (M+H+). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
76.5% | 4-Iodosalicylic acid 60 (7.3 g, 27.65 mmol) was dissolved in 41 ml DMF and NaHCO3 (2.78 g, 33.18 mmol) were added (evolution of CO2) and the mixture stirred for 5 min. MeI (2.66 ml, 5.85 g, 41.47 mmol, 1.5 eq) was added and the reaction mixture was heated to 40 C. for 5 h while stirring (monitored by TLC). Upon reaction completion, the mixture was diluted with 170 ml H2O and 170 ml EA. The organic layer was subsequently washed with 170 ml of 5% NaHCO3, 170 ml 5% NaCl and was dried over Na2SO4. The solvent was evaporated to give ?9 g of crude oily product (black color), which was purified by column chromatography: SiO2 (100 g), Hexane, Hexane:EA 100:2. 5.86 g, Yield: 76.5%. |
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