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CAS No. : | 89-69-0 | MDL No. : | MFCD00007072 |
Formula : | C6H2Cl3NO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 226.44 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P264-P270-P301+P312+P330-P501 | UN#: | N/A |
Hazard Statements: | H302 | 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 |
---|---|---|
70% | With KF In sulfolane; ethyl acetate | EXAMPLE 1 5-Chloro-2,4-difluoronitrobenzene (2) 200 g (0.883 mol) of 2,4,5-trichloronitrobenzene and 128.4 g (2.21 mol) of KF in 500 ml of tetramethylenesulfone were reacted at 200° C. under nitrogen for 3.5 hours. To the mixture was added 500 ml of ethyl acetate and the precipitate was filtered. The filtrate was washed with brine, dried over magnesium sulfate and concentrated. Distillation at 85°-90° C./0.9 mm afforded pure compound 2 with more than 70percent yield. 1 H-NMR from CDCl3 (δ ppm): 7.17(dd, 1H, J=8 Hz, 9 Hz), 8.26 (dd, 1H, J=7.5 Hz, 7.5 Hz). MS(m/z): 193 (M+). |
69% | With potassium fluoride; cesium fluoride In sulfolane | EXAMPLE 1 Preparation of 5-chloro-2,4-difluoronitrobenzene 452.8 g (2 mol) of 2,4,5-trichloronitrobenzene, 232.4 g (4.0 mol) of potassium fluoride, 60.8 g (0.4 mol) of cesium fluoride and 632 g of sulfolane are introduced into a 2 l three-necked flask with an internal thermometer, paddle mixer and reflux condenser. The reaction suspension is heated to 160° C. and stirred vigorously at this temperature for 8 hours. Subsequently it is cooled to room temperature, the precipitated salts are filtered off with suction and the crude solution is fractionally distilled. 267.1 g of 5-chloro-2,4-difluoronitrobenzene are obtained, corresponding to a yield of 69percent of theory. |