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CAS No. : | 147460-41-1 | MDL No. : | MFCD00040939 |
Formula : | C6H4BrFO | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | HUVAOAVBKOVPBZ-UHFFFAOYSA-N |
M.W : | 191.00 | Pubchem ID : | 2724600 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P305+P351+P338 | UN#: | |
Hazard Statements: | H227-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 |
---|---|---|
47% | To a solution of MgCl2 (powder 325 mesh, 0.734 g, 7.71 mmol, 2 eq), paraformaldehyde (0.347 g, 11.57 mmol, 3 eq) and Et3N (1.08 mL, 7.71 mmol, 2 eq) in THF (20 mL) was added 276 (0.800 g, 3.68 mmol, 1 eq), heated in the microwave at 160 C for 15 min. TLC (3:2 Hexane:DCM) showed complete consumption of 3. THF was evaporated and the reaction mixture was taken up in EtOAc, washed with brine, dried, filtered and concentrated in vacuo to afford 0.52 g of 277 which was used without purification. Yield 47% |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
58% | With caesium carbonate; In N,N-dimethyl-formamide; at 100.0℃; for 15.0h; | itermediteExthp1eI5. ?sulfOnamide ?,?a) .To a solutiOn of 2-brotho-5-fludrophenol (3g. 15.7 mmol) in DMF (5 ml) was added cesium carbonate (7.7 g, 23.56 mmol, 1.5 eq) and sodium chlorodifluoroacetate(6 g, 39.26 nimol;2:5 eq) and the reaction mixture was heated at 100C for 15 h. Thereaction mixture was then exttacted with Water and ethyl acetate (3 x 50 mI) Thecombined Organic layer was washed with water, brine and dried over sodium sulphate. The solvent was distilled off to afford the crude residue which was purified by column chromatography (60-120 silica ge110% ethyl acetate in hexane) in 58 % yield (2.2 g). |
With caesium carbonate; In water; N,N-dimethyl-formamide; at 100.0℃; for 15.0h; | Preparation Example 3 A mixture of 2-bromo-5-fluorophenol (3 g), sodium chlorodifluoroacetate (6 g), cesium carbonate (7.7 g), water (3 mL) and DMF (30 mL) was stirred under heating at an oil temperature of 100C for 15 hours. The reaction mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate. The organic layer was washed with 1M aqueous sodium hydroxide solution, further washed with water, dried and concentrated under reduced pressure to obtain 1-bromo-2-(difluoromethoxy)-4-fluorobenzene (2.77 g). | |
With water; caesium carbonate; In N,N-dimethyl-formamide; at 100.0℃; for 2.0h; | Intermediate Example Int 17.11 -Bromo-2-(dif luoromethoxy)-4-f luorobenzeneTo a stirred solution of 2-bromo-5-fluorophenol (21 .0 g) in DMF (600 mL) was added cesium carbonate (107.5 g), sodium chlorodifluoroacetate (52.3 g) and water (29.4 mL). The mixture was stirred at 100 C for 2 h. The mixture was filtrated and the resulting solution was extracted with pentane (4 x 400 mL). The combined organic layers were washed with saturated sodium chloride solution, dried (sodium sulfate) and the solvent was removed in vacuum, to give 7.14 g of the title compound as a crude product. Silica gel chromatography afforded 3.2 g of the title compound.1H-NMR (400MHz, DMSO-d6): delta [ppm] = 7.10 - 7.16 (m, 1 H), 7.34 (t, 1 H), 7.33 - 7.36 (m, 1 H), 7.79 (dd, 1 H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium carbonate; In N,N-dimethyl-formamide; at 90.0℃; | Compound 15 (80 g, 0.42 mol) was dissolved in DMF (800 mL), and sodium carbonate (266 g, 2.5 mol) wasadded. The temperature was increased to 90 C. Chlorodifluoroacetic acid (191 g, 1.46 mol) was added dropwise. Afterthe completion of addition, temperature was maintained at 90 C to react overnight. The reaction solution is cooled toroom temperature, poured slowly into ice water, and extracted twice with ethyl acetate. The organic phases were combined,washed once with saturated brine, dried over anhydrous sodium sulfate, and spin-dried to obtain 95 g of crudeproduct, which was used directly in the next reaction. 1H NMR (400 MHz, CDCl3): delta 7.62-7.58 (m, 1H), 7.04-7.01 (m,1H), 6.93-6.88 (m, 1H), 6.57 (t, J = 72.8 Hz, 1H); MS (ESI) (m/z): [M+H]+ 240.9. |
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