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CAS No. : | 348-59-4 | MDL No. : | MFCD00060656 |
Formula : | C6H3Cl2F | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | BJQTYCQGIXZSNM-UHFFFAOYSA-N |
M.W : | 164.99 | Pubchem ID : | 136173 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P210-P264-P280-P302+P352+P332+P313+P362+P364-P305+P351+P338+P337+P313-P403+P235-P501 | UN#: | N/A |
Hazard Statements: | H227-H315-H319 | Packing Group: | N/A |
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 |
---|---|---|
95% | General procedure: 14 Typical continuous diazotization procedure: Material A (50 mL of aqueous solution containing amine (100 mmol), fluoroboric acid (120 mmol), hydrochloric acid (180 mmol)), and material B (50 mL of aqueous solution containing sodium nitrite (105 mmol)) were pumped into the T-joint at 4 mL/min, respectively, after a residence time of about 15 s at 25 C in a reacting tube, the mixture flowed through the outlet and accumulated in the cooling vessel. Vigorous stirring was maintained. The solid was filtered with suction after the slurry was cooled to -5 C. The solid was washed with methanol and then dried in vacuo to yield the corresponding diazonium tetrafluoroborate. 15 Typical continuous fluorodediazoniation procedure: Slurry of the diazonium tetrafluoroborate prepared as above in 300 mL of cosolvent was introduced into a reacting tube continuously at a flow rate of 4 mL/min. The mixture was maintained for 1 min at setting temperature and then cooled in the tandem tube. The collected liquid was washed with aqueous NaOH and water, nearly colorless liquid was obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | With sulfuric acid; nitric acid; at 0 - 20℃; for 4.16667h; | To a solution of 1,4- dichloro-2-fluorobenzene (2.227 g, 13.5 mmol) in sulfuric acid (3.59 mL, 67.3 mmol) at 0C was added nitric acid (0.612 mL, 13.50 mmol) dropwise over 10 min. The reaction was stirred at rt for 4 h. The mixture was poured into ice water, extracted with EtOAc (150 mL). The extract was washed with water, saturated NaHCO3 solution and brine sequentially, dried over MgSO4, filtered and concentrated under vacuum. The residue was purified with a silica gel flash column, eluting with 0-20% EtOAc in hexane to afford 1,4- dichloro-2-fluoro-5-nitrobenzene (2.79 g, 13.29 mmol, 98 % yield) as a tan solid.1H NMR (CDCl3) d 7.40 (1H, d, J = 7.8 Hz), 8.09 (IH, d, J = 6.9 Hz). |
1.3 g | With nitric acid; trifluoroacetic acid; at 20℃; for 3h; | (Step 1) Synthesis of 1,4-dichloro-2-fluoro-5-nitrobenzene (0422) According to (Step 1) of Example 19, <strong>[348-59-4]1,4-dichloro-2-fluorobenzene</strong> (1.00 g) was dissolved instead of 1-chloro-2-fluoro-4-methylbenzene in TFA (10 mL). To the solution, fuming nitric acid (5.0 mL) was added dropwise. The mixture was stirred at room temperature for 3 hours, and then, the solution was added to an aqueous sodium bicarbonate solution. The precipitated solid was collected by filtration and dried to obtain 1.30 g of the title compound as a white solid. |
1.3 g | With nitric acid; trifluoroacetic acid; at 20℃; for 0.05h; | General procedure: 1-hloro-2-fluoro-4-methylbenzene (1.00 g) was dissolved in TFA (10 mL). The solution was cooled to 0C, and then, fuming nitric acid (5.0 mL) was added dropwise thereto. The mixture was stirred at 0C for 30 minutes, and then, the solution was added to an aqueous sodium bicarbonate solution and neutralized, followed by extraction with chloroform. The extract was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel chromatography (hexane/ethyl acetate) to obtain 1.31 g of the title compound as a white solid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
92% | With trichloroisocyanuric acid; bromine; In tetrachloromethane; at -10 - 100℃; for 18h;Photolysis; | General procedure: Round bottom flask equipped with Dimroth condenser (chilled to -10 C) was charged with arenecarboxylic acid (1.8 mmol), chloroisocyanurate, brominating agent and solvent (8 mL). The mixture was magnetically stirred and heated in an oil bath under 3 W LED warm-white lamp irradiation (LL) or under fluorescent room light irradiation (FL). The cooled reaction mixture was filtered through a short silica gel pad, washed with 1 M aq Na2SO3, dried over Na2SO4, filtered and the solvent was removed by distillation. In case of volatile product the yield was determined by gas chromatography (GC) with internal standard. The results are presented in Table 7 |
...presented by the following formula (4) which can respectively correspond to the formula (1) can be obtained. (D) Fluorine substituted aromatic compound represented by the formula (4) corresponding to the hydroxy compound wherein X1 is a substituent of the group (a) in the formula(1): ... 2,4-dinitrofluorobenzene, 2,5-dinitrofluorobenzene, 2,4,6-trinitrofluorobenzene, 2-cyanofluorobenzene, 3-cyanofluorobenzene, 4-cyanofluorobenzene, 2-chlorofluorobenzene, 3-chlorofluorobenzene, 4-chlorofluorobenzene, 2,4-dichlorofluorobenzene, 2,5-dichlorofluorobenzene, 2,6-dichlorofluorobenzene, 3,4-dichlorofluorobenzene, 3,5-dichlorofluorobenzene, 2,4,6-trichlorofluorobenzene, 2,4,5-trichlorofluorobenzene, pentachlorofluorobenzene, ... |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogenchloride; sodium hydrogencarbonate; potassium carbonate; In water; ethyl acetate; acetone; | EXAMPLE 19 2-[3-(2,5-Dichloro-phenoxy)4-ethyl-phenyl]-N-(4-sulfamoyl-phenyl)-acetamide (I-19) step 1-To a solution of 12a (0.200 g; 0.960 mmol) and NMP (4 mL) was added K2CO3 (0.398 g; 2.88 mmol) and <strong>[348-59-4]1,4-dichloro-2-fluoro-benzene</strong> (0.124 mL; 1.056 mmol). The reaction was heated to 120 C. and monitored by TLC. After 8 h the reaction was cooled to RT and 10% HCl was added. The mixture was extracted with EtOAc and the combined extracts were washed with H2O and brine. The extracts were dried (Na2SO4) filtered and evaporated. The crude product was purified by SiO2 chromatography eluding with a gradient of hexane/EtOAc (100:0 to 60:40) to afford 142. steps 2 and 3-Hydrolysis and formation of the acid chloride were carried as described in step 7and 8 of Example 1 and used without additional purification. step 4-The acid chloride from step 3 (0.415 mmol) was dissolved in acetone (2 mL) and the flask and purged with nitrogen. NaHCO3 (0.070 g; 0.83 mmol) was added followed by 4-amino-benzenesulfonamide (0.072 g; 0.415 mmol) and water (4 mL). The mixture was sonicated for 5 min and allowed to stir for 12 h at RT. The reaction mixture was filtered and the crude product was washed sequentially with water and diethyl ether to afford I-19 Compound I-21 was prepared in the same manner except 4-amino-benzenesulfonamide was replaced with 2-chloro-phenylamine. |
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