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CAS No. : | 289039-82-3 | MDL No. : | MFCD00144772 |
Formula : | C8H6ClIO2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | LNCNRPALSKTJBG-UHFFFAOYSA-N |
M.W : | 296.49 | Pubchem ID : | 23510379 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302 | 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% | A solution of <strong>[13421-00-6]5-chloro-2-iodo<strong>[13421-00-6]benzoic acid</strong></strong> (3.0 g, 10.62 mmol), SOC12 (12 mL) and DMF (0.6 mL) was gently warmed with a heat gun until the mixture becamehomogeneous (15 mm). The solution was maintained at 23C for additional 30 mm and then the solution was concentrated. MeOH (24 mL) was added to the crude residue and the solution was maintained at 23C for 30 mm. The solution was concentrated and the residue was purified by flash chromatography on Biotage silica gel cartridge (cyclohexane to cyclohexane : EtOAc = 85 : 15) to afford methyl 5-chloro-2-iodobenzoate (3.02 g, 10.20 mmol, 96%).UPLC-MS: 1.17 mm, 296.6 [M+H]+, method 12. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | With sodium hydrogencarbonate; In N,N-dimethyl-formamide; at 20℃; for 24h; | To a round bottom flask was added NaHCO3 (22.3 g, 266 mmol), <strong>[13421-00-6]5-chloro-2-iodo<strong>[13421-00-6]benzoic acid</strong></strong> (25.0 g, 89.0 mmol), DMF (88 mL), and Mel (11.1 mL, 177 mmol) and the reaction was stirred at room temperature. After 24 h, the reaction was partitioned between water and EtOAc. The aqueous phase was extracted with EtOAc (2x). The combined organic extracts were washed with water (3x), brine, dried over Na2SO4, and concentrated. The crude residue was purified via Biotage to afford methyl 5-chloro-2-iodobenzoate (25.8 g, 87.0 mmol, 98% yield). LC/MS m/z 297 [M+H]+ |
With sodium hydrogencarbonate; In N,N-dimethyl-formamide; at 20℃; | [00392] chi0 a round bottomed flask was added NaHC03 (22.31 g, 266 mmol), <strong>[13421-00-6]5-chloro-2-iodo<strong>[13421-00-6]benzoic acid</strong></strong> (25 g, 89 mmol), DMF, and Mel (11.07 mL, 177 mmol). The reaction was stirred at room temperature overnight. The reaction was diluted with water and EtOAc. The layers were separated and the aqueous layer was extracted with EtOAc. The combined organic layers were washed with water (3x) and brine before being dried over Na2S04, filtered, and concentrated. The crude residue was purified via Biotage to afford the titled compound (25.81 g, 87 mmol). LC/MS m/z 291[M+H]+. |
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