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CAS No. : | 1003709-39-4 | MDL No. : | MFCD09263434 |
Formula : | C8H6BrFO2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | UVSGTNJGIMPLAM-UHFFFAOYSA-N |
M.W : | 233.03 | Pubchem ID : | 45073546 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-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 |
---|---|---|
74% | With N-Bromosuccinimide; dibenzoyl peroxide; In acetonitrile; for 4.0h;Reflux; | A mixture of 2-bromo-4-fluoro-5-methyl-benzoic acid (0.5 g, 2.14 mmol), N-bromosuccinimide (381 mg, 2.15 mmol) and benzoyl peroxide (10 mg, 0.04 mmol) in CH3CN (10 mL) was heated at reflux for 4 h. The reaction mixture was cooled to 0 C and 5% aqueous Na2S203 was added. The CH3CN was evaporated and the residue was extracted with EtOAc (3 x 100 mL). The combined organic phases were dried (Na2S04), filtered, and evaporated. The residue was purified by chromatography (silica gel, 2-20% EtOAc/hexane) to give 2-bromo-5-bromomethyl- 4-fluoro-benzoic acid (500 mg, 74%). MS calcd. for C8H6Br2F02 [(M-H) ] 309, obsd. 308.6. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
93% | With sodium chlorite; potassium dihydrogenphosphate; aminosulfonic acid; In 1,4-dioxane; water; at 20.0℃; | A mixture of 2-bromo-4-fluoro-5-methyl-benzaldehyde (available from 3B Scientific Corporation, 1840 Industrial Drive, Suite 160, LibertyviUe, IL 60048, USA; 1.0 g, 4.61 mmol), sulfamic acid (2.68 g, 27.65 mmol), sodium chlorite (539 mg, 6 mmol) and KH2P04 (7.52 g, 55.3 mmol) in 50% aqueous dioxane (96 mL) was stirred at room temperature overnight. The reaction mixture was concentrated, and water (20 mL) was added. The resulting mixture was extracted with EtOAc (3 x 250 mL). The combined organic layers were dried (Na2S04), filtered, and evaporated to give 2-bromo-4-fluoro-5-methyl-benzoic acid (1.0 g, 93%) as an off-white solid. MS calcd. for C8H7BrF02 [(M-H) ] 231, obsd. 231.0. |
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