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CAS No. : | 1516-96-7 | MDL No. : | MFCD12024327 |
Formula : | C15H23BrO | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | KKHJQLVAMOKQHO-UHFFFAOYSA-N |
M.W : | 299.25 | Pubchem ID : | 13691541 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | N/A |
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 |
---|---|---|
Reference Example 2To a 500 mL round-bottom four-neck flask equipped with a Dimroth condenser with a nitrogen introducing tube attached thereto, a thermometer, a magnetic rotator and a dropping funnel were added 25.25 g of 4-hydroxy-3,5-di-tert-butylbromobenzene and 250.0 mL of dehydrated dimethylformamide. The resulting mixture was cooled to -41 C., and 4.82 g of 60% by weight sodium hydride was added at -40 to -50 C. The resulting mixture was stirred at -40+/-2 C. for 2 hours to allow to react. To the resulting reaction mixture was added dropwise 7.60 mL of methyl iodide at the same temperature. The temperature of the resulting mixture was raised to 4 C. over 4.5 hours. The resulting reaction mixture was stirred at room temperature overnight, and poured into 500 g of ice water. The resulting mixture was extracted with 200 mL of ethyl acetate three times. The resulting organic layers were mixed, and dried with anhydrous magnesium sulfate. After magnesium sulfate was removed by filtration, the resulting filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane) to obtain 25.30 g of a colorless crystal of 4-methoxy-3,5-di-tert-butylbromobenzene.Purity (GC): 99.9%GC-MS m/z: 300, 298 (calculated value of the molecular weight: 299.25) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95.2% | With potassium carbonate; In acetone; at 22℃; for 13h;Heating / reflux; | Reference Example 6 4-bromo-2,6-di-tert-butylanisole Under an argon atmosphere, to a solution of <strong>[1139-52-2]4-bromo-2,6-di-tert-butylphenol</strong> (50 g, 0.175 MoL) and potassium carbonate (96.7 g, 4.0 equivalents) in acetone (750 ML) was added dimethyl sulfate (38.6 g, 1.75 equivalents) at 22C, and the mixture was stirred under reflux for 13 hrs.. Insoluble materials were filtered off and the solvent was evaporated under reduced pressure.. ethyl acetate (150 ML) and water (100 ML) were added, the mixture was partitioned, and the organic layer was washed successively with water (100 ML), 5% aqueous NaHCO3 solution (100 ML) and 5% aqueous NaCl solution (100 ML).. The organic layer was dried over anhydrous magnesium sulfate, filtered by gravity, and the filtrate was concentrated under reduced pressure to give the title compound (56.1 g, brown oil).. yield 95.2%1H-NMR (300MHz, CDCl3, TMS) delta: 1.41 (s, 18H), 3.68 (s, 3H), 7.33 (s, 2H). |
95.2% | With potassium carbonate; In acetone; at 22℃; for 13h;Heating / reflux; | Reference Example 2 4-Bromo-2,6-di-tert-butylanisole Under argon atmosphere, to a solution of <strong>[1139-52-2]4-bromo-2,6-di-tert-butylphenol</strong> (50 g, 0.175 mol) and potassium carbonate (96.7 g, 4.0 equivalents) in acetone (750 mL) was added dimethyl sulfate (38.6 g, 1.75 equivalents) at 22C. The mixture was stirred under reflux for 13 hours. Insoluble substances were filtered off and the solvent was distilled off under reduced pressure. By adding ethyl acetate (150 mL) and water (100 mL) to the residue, the reaction mixture was allowed to separate into layers. An organic layer was washed successively with water (100 mL), a 5% NaHCO3 aqueous solution (100 mL) and a 5% NaCl aqueous solution (100 mL), dried over anhydrous magnesium sulfate and then naturally filtered. The filtrate was concentrated under reduced pressure to obtain the title compound (56.1 g, brown oil). Yield 95.2%. 1H-NMR (300 MHz, CDCl3, TMS) delta: 1.41 (s, 18H), 3.68 (s, 3H), 7.33 (s, 2H). |
89% | With sodium hydride; In tetrahydrofuran; at 75℃; for 12h; | To a 500 mL flask was added 200 ml of THF, NaH (3.2 g, 131.5 mmol), and a solution of <strong>[1139-52-2]4-bromo-2,6-di-tert-butylphenol</strong> (25 g, 87.7 mmol) in THF.Dimethyl sulfate (9.1 ml, 96.4 mmol) was added dropwise and stirred at 75 C for 12 h.Cool to room temperature, add 100 ml of water to quench, extract with EA, dry the organic phase, concentrate, and obtain the product by column chromatography(Colorless liquid, 23.4 g, yield = 89%). |
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