Structure of 1139-52-2
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The BI-3802 was designed by Boehringer Ingelheim and could be obtained free of charge through the Boehringer Ingelheim open innovation portal opnMe.com, associated with its negative control.
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CAS No. : | 1139-52-2 |
Formula : | C14H21BrO |
M.W : | 285.22 |
SMILES Code : | OC1=C(C(C)(C)C)C=C(Br)C=C1C(C)(C)C |
MDL No. : | MFCD00051598 |
Boiling Point : | No data available |
InChI Key : | SSQQUEKFNSJLKX-UHFFFAOYSA-N |
Pubchem ID : | 70829 |
GHS Pictogram: |
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Signal Word: | Warning |
Hazard Statements: | H315-H319-H335 |
Precautionary Statements: | P261-P305+P351+P338 |
* 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) |
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