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CAS No. : | 858854-82-7 | MDL No. : | MFCD08166414 |
Formula : | C6H4ClIO | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | CBGCAUCBOPFLFN-UHFFFAOYSA-N |
M.W : | 254.45 | Pubchem ID : | 12175702 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | 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 |
---|---|---|
100% | With ethanol; sodium hydroxide; at 25℃; for 2h;Inert atmosphere; Reflux; | (c) Step 3 Sodium hydroxide (32.0 g, 800 mmol) was added at 25 C. to 400 mL of an ethanol solution of 3-chloro-2-iodophenyl N,N-diethylcarbamate (57.0 g, 161 mmol), and the reaction solution was heated and refluxed for two hours. The ethanol was distilled off under reduced pressure, and the residue was dissolved in 400 mL of water and extracted by petroleum ether. The water layer was neutralized by 2N hydrochloric acid, and extracted by ethyl acetate. The combined organic layers were washed with (saturated) brine, dried with anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to obtain 3-chloro-2-iodophenol (41.0 g, quantitative). 1H NMR (400 MHz, CDCl3) delta 5.58 (brs, 1H), 6.90 (dd, J=1.2, 8.4 Hz, 1H), 7.06 (dd, J=1.2, 8.0 Hz, 1H), 7.21 (t, J=8.0 Hz, 1H). |
Carbamate 185 (10 g, 28 mmol, 1 eq) was treated with sodium hydroxide (11 g, 283 mmol, 10 eq) in refluxing ethanol (140 mL). After 14 h, the solution was allowed to cool to rt, acidified with HCl 6N then extracted with DCM (3×60 mL). The combined organics were dried over Na2SO4, filtered and concentrated. The residue was purified by flash chromatography (Hexane/DCM 0% to 100%) to obtain 186 an oil (3.75 g, 15 mmol). Yield 52%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
97% | With potassium carbonate; In acetone; for 5h;Inert atmosphere; Reflux; | (d) Step 4 Potassium carbonate (26.7 g, 194 mmol) and tert-butyl bromoacetate (34.6 g, 177 mmol) were added to 400 mL of an acetone solution of <strong>[858854-82-7]3-chloro-2-iodophenol</strong> (41.0 g, 161 mmol), and heated and refluxed for five hours. The reaction solution was filtered, and the crude product obtained by concentrating the filtrate was purified by silica gel chromatography (ethyl acetate/petroleum ether), and tert-butyl 2-(3-chloro-2-iodophenoxy)acetate (58.0 g, 97%) was obtained. 1H NMR (400 MHz, CDCl3) delta 1.50 (s, 9H), 4.61 (s, 2H), 6.58 (dd, J=1.2, 8.0 Hz, 1H), 7.15 (dd, J=1.2, 8.0 Hz, 1H), 7.23 (t, J=8.0 Hz, 1H). |
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