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CAS No. : | 2252-37-1 | MDL No. : | MFCD01569539 |
Formula : | C7H4BrFO2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | MDAZJVAIZVUWDE-UHFFFAOYSA-N |
M.W : | 219.01 | Pubchem ID : | 302621 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P301+P312-P302+P352-P304+P340-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 |
---|---|---|
85% | With sulfuric acid; at 80℃; for 12h; | Step 1 : Synthesis of methyl 2-bromo-6-fluorobenzoate (2).[00363] 2-Bromo-6-fluorobenzoic acid (1, 12.50 g, 57 mmol) was dissolved in a mixture of methanol (60 mL) and cone, sulfuric acid (65 mL). The solution was heated to 80 C and stirred for 12 h. The reaction mixture was cooled and 20% sodium carbonate solution (500 mL) was added slowly to reach pH = 8. The mixture was extracted with dichloromethane (3 x 180 mL), and the combined organic layers were dried over magnesium sulfate and evaporated. The title compound (11.29 g, 48.5 mmol, 85%) was obtained as a brown oil. |
85% | With sulfuric acid; at 80℃; for 12h; | [00499] 2-Bromo-6-fluorobenzoic acid (37) (12.50 g, 57 mmol) was dissolved in a mixture of methanol (60 mL) and cone, sulfuric acid (65 mL). The solution was heated to 80 C and stirred for 12 h. The reaction mixture was cooled and 20% sodium carbonate solution (500 mL) was added slowly to reach pH = 8. The mixture was extracted with dichloromethane (3 x 180 mL), and the combined organic layers were dried over magnesium sulfate and evaporated. The title compound (11.29 g, 48.5 mmol, 85%) was obtained as a brown oil. |
63% | With sulfuric acid; at 80℃; for 12h; | Asolution containing 2-bromo-6-fluorobenzoic acid (1.0equiv, 0.30 g, 1.37 mmol) and sulfuric acid (1.6 mL) in methanol (1.4 mL) washeated at 80 C for 12 h. The reaction was quenched with satd. aqueous Na2CO3until pH 8, and the aqueous phase was extracted with CH2Cl2(2 x 10 mL). The combined organic extracts were washed with water (20 mL),brine (20 mL), dried over Na2SO4 and filtrated.Evaporation of the solvent under reduced pressure followed by flashchromatography (SiO2, 95/5 hexane/EtOAc) afforded 200 mg (63%) ofthe entitled ester as a yellow oil. 1H-NMR (400 MHz, CDCl3, 25 C): d 7.40 (ddd, J = 8.3, 0.8, 0.8Hz, 1H), 7.27 (ddd, J = 8.3, 8.3, 5.8Hz, 1H), 7.09 (ddd, J = 8.8, 8.3, 0.8 Hz, 1H), 3.98 (s, 3H) ppm. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With caesium carbonate; In acetonitrile; | 17.1 Ethyl 2-bromo-6-fluorobenzoate To a solution of 2-bromo-6-fluoro-benzoic acid (5 g, 22.83 mmol) and Cs2CO3 (14.9 g, 45.7 mmol) in CH3CN (100 mL) was added CH3CH2I (7.12 g, 45.7 mmol) dropwise. The mixture was stirred at 30 C. overnight. The mixture was filtered and the filtrate was concentrated. The residue was purified by silica gel column chromatography, eluting with PE/EA (10:1) to give the title compound as a colorless oil (2 g, 25%). LCMS (ESI+): m/z 247.249. (M+H)+, Rt: 0.93 min. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
99.7% | With potassium carbonate; In N,N-dimethyl-formamide; at 20℃; for 4h; | To a solution 2-bromo-6-fluorobenzoic acid (50 g, 0.229 mol) and potassium carbonate (31.6 g, 0.229 mol) in N,N-dimethylformamide (250 mL) was added dropwise methyl iodide (51.83 g, 0.365 mol) over a 30 minute period. The reaction mixture was stirred at RT for 3.5 hours. The resulting mixture was diluted with water (500 mL) and extracted with EtOAc (3*300 mL). The combined organic layers were washed with 1M aqueous HCl (100 mL), dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure to give the title compound (53 g, 99.7%). |
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