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CAS No. : | 602-94-8 | MDL No. : | MFCD00002406 |
Formula : | C7HF5O2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | YZERDTREOUSUHF-UHFFFAOYSA-N |
M.W : | 212.07 | Pubchem ID : | 11770 |
Synonyms : |
|
Signal Word: | Warning | Class: | |
Precautionary Statements: | P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | 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 |
---|---|---|
52% | Weigh 24mg pentafluorobenzoic acid, 42mg HATU, 15mg HOAT in a 25ml round bottom flask and add 0.8mlDCM, 0.2 ml of DMF and 33 mul of DIEA as solvents were stirred at room temperature for about 10 minutes. 37 mg of the A1 intermediate was added to the reaction system. After stirring at room temperature for about 1 hour, 100 ml of saturated aqueous sodium bicarbonate solution was added, followed by 15 ml of DCM. The mixture was extracted 3 times and the resulting organic phase was dried under reduced pressure. The residue was applied to a silica gel column with DCM:MeOH=70:1 (v/v) to give 29 mg of the compound represented by Formula III-3 in 52% yield. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
91% | With magnesium hydroxide; N-benzyl-N,N,N-triethylammonium chloride; potassium hydroxide; In water; at 120℃; for 3h; | Add 212g of 2,3,4,5,6-pentafluorobenzoic acid and 600g of water to the reaction kettle, turn on stirring, add 367g of 30% potassium hydroxide aqueous solution at room temperature, and then add 65g of benzyltriethylammonium chloride with 60g of magnesium hydroxide, heated to 120C, refluxed for 3 hours, cooled, filtered, the filter cake was washed with water 3 times, the filtrate was neutralized with hydrochloric acid to pH=2, extracted with ether three times, and the extract was concentrated to obtain 4-hydroxy-2,3,5,6-tetrafluorobenzoic acid solid is 189.3g, the content detected by HPLC is over 98%, and the yield is 91%. |
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