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CAS No. : | 132794-07-1 | MDL No. : | MFCD00077480 |
Formula : | C7H3ClF2O2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | PEPCYJSDHYMIFN-UHFFFAOYSA-N |
M.W : | 192.55 | Pubchem ID : | 2733274 |
Synonyms : |
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Signal Word: | Danger | Class: | |
Precautionary Statements: | P280-P305+P351+P338-P403-P501 | UN#: | |
Hazard Statements: | H318 | 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 |
---|---|---|
94% | sulfuric acid; for 18h;Heating / reflux; | Sulfuric acid (62.4 ml, 1.13 moles) was added to a solution of <strong>[132794-07-1]2,5-difluoro-4-chloro-benzoic acid</strong> (750.0 g, 3.895 moles) (PLEASE DEFINE THE SOURCE OF THIS REACTANT) in absolute ethanol (3.75 L). The mixture was refluxed for 18 hours. The mixture was concentrated to remove most of ethanol and then cooled to room temperature. The residue was neutralized with 1N aqueous NaOH (2.4 L) and extracted with ethyl acetate (2×1L). The combined extracts were washed with sat. aqueous NaHCO3 and brine, then dried with (MgSO4) and concentrated to dryness. Ethyl 2,5-difluoro-4-chloro-benzoate (806.7 g) was obtained at 94% yield. 1H NMR (in CDCl3): delta7.72 (dd, J=9.1/6.2, 1H), 7.22 (dd, J=9.1/5.6, 1H), 4.39 (q, 3J=7.0, 2H), 1.39 (t, J=7.0, 3H). GC-MS: 161 (M+). |
With sulfuric acid; for 72h;Heating / reflux; | Preparation 1 4-Chloro-2,5-difluoro-benzaldehyde <strong>[132794-07-1]4-Chloro-2,5-difluoro-benzoic acid</strong> (25.0 g, 129.84 mmol), H2SO4 (3.46 mL, 64.92 mmol) and EtOH (300 mL) were combined and heated at reflux for 72 h. The solution was cooled, concentrated, diluted with H2O (1.0 L), and extracted with EtOAc (3*500 mL). The combined organic extracts were washed with saturated NaHCO3 (3*200 mL), H2O (200 mL), dried (MgSO4), filtered, and concentrated to provide 28.17 g of <strong>[132794-07-1]4-chloro-2,5-difluoro-benzoic acid</strong> ethyl ester as a golden oil. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
PREPARATION 151 4-Chloro-2,5-difluoro-N-(3,4-dimethoxybenzyl)benzamide (1.66 g) was obtained from <strong>[132794-07-1]4-chloro-2,5-difluorobenzoic acid</strong> (1.05 g) and veratrylamine (0.91 mL) in a in a manner similar to preparation 1. NMR (DMSO-d6, delta): 3.73 (3H, s), 3.74 (3H, s), 4.39 (2H, d, J=6 Hz), 6.81-6.97 (3H, m), 7.67 (1H, dd, J=6, 9 Hz), 7.79 (1H, dd, J=6, 9 Hz), 8.96 (1H, t, J=6 Hz). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
79% | EXAMPLE 2 The above reaction was repeated, cutting down the reflux time to 2 hours instead of 18 hours. The conversion was 79% and the yield of 4-chloro-2,5-difluorobenzoic acid was 83%. |