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CAS No. : | 261723-33-5 | MDL No. : | MFCD09263985 |
Formula : | C7H6BrFO | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | HHGJENWYHVFPSA-UHFFFAOYSA-N |
M.W : | 205.02 | Pubchem ID : | 44181801 |
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 |
---|---|---|
100% | PREPARATION 7 1-Bromo-3-fluorobenzyl alcohol To 1-bromo-3-fluorobenzaldehyde (1.60 kg, 7.91 mol) in methanol (14 L) at 0° C. add sodium borohydride (284 g, 7.93 mol) in portions over 30 min to control the exotherm and gas evolution. After 15 min, quench with water (500 mL) and concentrate to obtain a yellow oil. Dissolve the oil in ethyl acetate (6 L) and wash with water (3 L). Extract the aqueous layer with ethyl acetate (1 L). Wash the combined organic phases with brine (2 L), dry over sodium sulfate, filter, and concentrate to obtain the title compound as an orange oil (1614 g, 100percent). 1H NMR (CDCl3) delta 7.40 (d, 1H), 7.18 (m, 1H), 7.07 (t, 1H), 4.86 (s, 2H). | |
With methanol; sodium tetrahydroborate; for 1h;Cooling with ice; | 9.1(2-Bromo-6-fluorophenyl)methanol20.0 g (0098 mol) of 2-bromo-6-fluorobenzaldehyde are dissolved in 500 ml of methanol and cooled in an ice bath; 3.72 g (0.098 mol) of sodium borohydride are then added thereto, portionwise.The mixture is stirred under cold conditions for 1 hour and the solvent is then evaporated off under reduced pressure.The residue is taken up between water and dichloromethane, and the organic phase is separated, dried and concentrated under reduced pressure.The residue is crystallized from pentane. 18.1 g of compound are obtained.1H NMR (CDCl3, delta in ppm): 2.15 (t, 1H); 4.95 (d, 2H); from 7.05 to 7.3 (m, 2H); 7.45 (d, 1H). | |
With methanol; sodium tetrahydroborate; for 1h;Cooling with ice; | 14.1(2-Bromo-6-fluorophenyl)methanol20.0 g (0.098 mol) of 2-bromo-6-fluorobenzaldehyde are dissolved in 500 ml of methanol and cooled in an ice bath; 3.72 g (0.098 mol) of sodium borohydride are then added portionwise thereto.The mixture is stirred under cold conditions for 1 hour and then the solid is evaporated under reduced pressure.The residue is taken up between water and dichloromethane and the organic phase is separated, dried and concentrated under reduced pressure.The residue is crystallised from pentane. 18.1 g of compound are obtained.1H NMR (CDCl3, delta in ppm): 2.15 (t, 1H); 4.95 (d, 2H); from 7.05 to 7.3 (m, 2H); 7.45 (d, 1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
83% | With pyridine; phosphorus tribromide; In chloroform; at 0 - 20℃; | PREPARATION 8 1-Bromo-3-fluorobenzyl bromide To a solution of <strong>[261723-33-5]1-bromo-3-fluorobenzyl alcohol</strong> (1.61 kg, 7.85 mol) in chloroform (14 L) at 0° C. add pyridine (770 mL, 9.52 mol) in one portion (slight exotherm) and stir at 0° C. for 5 min. Add phosphorus tribromide (900 mL, 9.49) dropwise while maintaining the internal temperature below 20° C. and stir the resulting solution overnight while allowing to warm to room temperature. Cool the reaction to 0° C. and quench slowly with ice water (2 L). Transfer to a 50 L flask, separate the layers and then extract the aqueous layer with chloroform (1 L). Wash the combined organic phases with 5percent sulfuric acid (2 L), saturated aqueous sodium bicarbonate (2 L), brine (2 L), dry over magnesium sulfate, filter, and concentrate to obtain the title compound as a yellow oil (1753 g, 83percent). 1H NMR (CDCl3) delta 7.43 (d, 1H), 7.21 (m, 1H), 7.09 (t, 1H), 4.68 (s, 2H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With thionyl chloride;N,N-dimethyl-formamide; In toluene;Cooling with ice; | After dissolving <strong>[261723-33-5](2-bromo-6-fluorophenyl)methanol</strong> (CAS 261723-33-5) (4.07 g) in toluene (50 ml), thionyl chloride (2.21 ml) was added dropwise while stirring on ice. N,N-Dimethylformamide (0.1 ml) was then added and the mixture was stirred for 6 hours. The reaction mixture was diluted with water, a 1N aqueous solution of sodium hydroxide was added and extraction was performed with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. After filtration, the solvent was distilled off under reduced pressure to obtain the title compound (4.45 g).1H-NMR (400 MHz, CDCl3); delta 4.77 (s, 2H), 7.04-7.20 (m, 2H), 7.38-7.41 (m, 1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With 1H-imidazole; In tetrahydrofuran; for 16h; | 9.2(2-Bromo-6-fluorobenzyloxy)-tert-butyldimethylsilaneIn a 500 ml round-bottomed flask, 15.7 g (0.076 mol) of the compound obtained previously are dissolved in 230 ml of THF, and 7.8 g (0.115 mol) of imidazole are added, followed by 13.8 g (0.092 mol) of tert-butyldimethylsilane chloride, and the reaction mixture is stirred for 16 hours.The solvent is then evaporated off under reduced pressure, the residue is taken up between water and diethyl ether, the resulting product is separated by settling out, and the organic phase is washed with water and dried over sodium sulphate.After evaporation of the solvent, 25 g of oil are recovered.1H NMR (CDCl3, delta in ppm): 0.0 (s, 6H); 0.8 (s, 9H); 4.7 (s, 2H); from 6.8 to 7.05 (m, 2H); 7.25 (d, 1H). | |
With 1H-imidazole; In tetrahydrofuran; for 16h; | 14.2 (2-Bromo-6-fluorobenzyloxy(tert-butyl)dimethylsilane15.7 g (0.076 mol) of the compound obtained above are dissolved in 230 ml of THF in a 500 ml round-bottomed flask, 7.8 g (0.115 mol) of imidazole and then 13.8 g (0.092 mol) of tert-butyldimethylchlorosilane are added and the reaction mixture is stirred for 16 hours.The solvent is then evaporated under reduced pressure, the residue is taken up between water and diethyl ether, separation by settling is carried out and the organic phase is washed with water and dried over sodium sulphate.After evaporating the solvent, 25 g of oil are collected.1H NMR (CDCl3, delta in ppm): 0.0 (s, 6H); 0.8 (s, 9H); 4.7 (s, 2H); from 6.8 to 7.05 (m, 2H); 7.25 (d, 1H). |
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