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CAS No. : | 940054-48-8 | MDL No. : | MFCD20646110 |
Formula : | C7H5ClFNO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 189.57 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Class: | ||
Precautionary Statements: | UN#: | ||
Hazard Statements: | Packing Group: |
* 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 |
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Stage #1: 4-chloro-6-fluoro-1H-indole-2,3-dione; 6-chloro-4-fluoro-1H-indole-2,3-dione With sodium hydroxide; dihydrogen peroxide In water at 0 - 20℃; Stage #2: With formic acid In water | 1.5 Stage 5: 2-amino-6-chloro-4-fluoro-benzoic acid (main isomer) and 2-amino-4-chloro-6-fluoro-benzoic acid (lesser isomer) First sodium hydroxide (10.7 g, 267 mmol) and then 30% hydrogen peroxide (10.7 ml) in water (96 ml) were added to a suspension of the product mixture from stage 4 (8.00 g, 40 mmol) in water (200 ml) at 0° C. The mixture was stirred at room temperature overnight and then brought to pH 3.3 with formic acid (approx. 20 ml, severe foaming). The title compound which had precipitated out was filtered off and dried over phosphorus pentoxide in vacuo. The aqueous solution was extracted with ethyl acetate (2*150 ml). The pH of the aqueous phase was corrected to 3.3 and extraction was carried out again with ethyl acetate (150 ml). The combined organic phases were dried with sodium sulfate and concentrated and the residue was dried in vacuo. Yield: 7.30 g (95%) of the mixture of the regioisomers in the ratio of 9:1, brown solid. |