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CAS No. : | 3337-59-5 | MDL No. : | MFCD00016419 |
Formula : | C8H6Cl2O3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | UKMOOQFHBGTLAO-UHFFFAOYSA-N |
M.W : | 221.04 | Pubchem ID : | 76856 |
Synonyms : |
|
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 |
---|---|---|
84.9% | With toluene-4-sulfonic acid; for 6h;Reflux; | [0246] 62.1 g (0.30 mol) of <strong>[3336-41-2]4-hydroxy-3,5-dichlorobenzoic acid</strong> was dissolved in 300 mL of methanol. 3 g of p-toluenesulfonic acid was added. The reaction mixture was heated and refluxed for 6 hours. The solvent was removed under reduced pressure. The residue was dissolved in 500 mL of dichloromethane, washed with water three times (200 mL3), and dried over anhydrous magnesium sulfate. The desiccant was removed by filtration, and the solvent was removed to obtain 56.3 g of the target product with a yield of 84.9%. m/z 219.01(M-H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | Step 1: Methyl 3,5-dichloro-4-hydroxybenzate. To a suspension of 5.00 g (24.2 mmol) of <strong>[3336-41-2]3,5-dichloro-4-hydroxybenzoic acid</strong> in 50 ml of MeOH was stirred in a 0 C. ice bath under Ar, 5.0 ml (68.5 mmol) of thionyl chloride was added over a period of 20 min. The reaction mixture was stirred for 1.5 hours more, then warmed to room temperature overnight. The mixture was extracted with EtOAc, washed with brine, and water, dried (MgSO4), filtered, and concentrated to afford a white solid (5.26 g, 98% yield): m.p. 117-119 C.: Rf 0.69 (40% EtOAc/hexane); 1H NMR (400 MHz, CDCl3) delta3.91 (s, 3, CH3), 6.28 (s, 1, OH), 7.97 ppm (s, 2, ArH). |
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