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CAS No. : | 39478-78-9 | MDL No. : | MFCD00800678 |
Formula : | C7H8BrN | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | RXQNKKRGJJRMKD-UHFFFAOYSA-N |
M.W : | 186.05 | Pubchem ID : | 2734805 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302+H312+H332-H315-H319-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 |
---|---|---|
51% | 5-Bromo-2-methylphenol; A solution of concentrated sulphuric acid (6 mL) in distilled water (75 mL) was added to 5-bromo-2-methylaniline (1 g, 5.38 mmol). The resultant suspension was heated to 90 C. and stirred for 4.5 h. The reaction mixture was then cooled using an ice bath and a solution of sodium nitrite (384 mg, 5.57 mmol) in water (5 mL) was added to the reaction mixture at 0 C. The reaction was then allowed to warm to ambient temperature. The reaction mixture was then added to a solution of concentrated sulphuric acid (6 mL) in water (75 mL) which had been preheated to 90 C. The reaction mixture was stirred for 1 h at 90 C. and allowed to cool, on standing, overnight. A precipitate was observed in the reaction mixture. The precipitate was collected by filtration, washed with water, and dried in a vacuum oven to afford 5-bromo-2-methylphenol as a brown solid (510 mg, 2.73 mmol, 51%). M.S. (ESI) (m/z) 185, 187[M-H]- | |
51% | A solution of concentrated sulphuric acid (6ml_) in distilled water (75ml_) was added to 5- bromo-2-methylaniline (1g, 5.38mmol). The resultant suspension was heated to 9O0C and stirred for 4.5h. The reaction mixture was then cooled using an ice bath and a solution of sodium nitrite (384mg, 5.57mmol) in water (5ml_) was added to the reaction mixture at O0C. The reaction was then allowed to warm to ambient temperature. The reaction mixture was then added to a solution of concentrated sulphuric acid (6ml_) in water (75ml_) which had been preheated to 9O0C. The reaction mixture was stirred for 1 h at 9O0C and allowed to cool, on standing, overnight. A precipitate was observed in the reaction mixture. The precipitate was collected by filtration, washed with water, and dried in a vacuum oven to afford 5-bromo-2-methylphenol as a brown solid (510mg, 2.73mmol, 51 %). M.S. (ESI) (m/z) 185, 187[M-H]- |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66% | With sodium carbonate;tetrakis(triphenylphosphine) palladium(0); In 1,2-dimethoxyethane; water; for 7h;Reflux; | (i) N-(3'-amino-4'-methylbiphenyl-4-yl)acetamido; 0.60 g (3.20 mmol) of 5-bromo-2-methylaniline and 1.01 g (4.87 mmol) of 4-acetamidophenylboronic acid pinacol ester were dissolved in 15 mL of DME. Next, 5 mL of a 2M aqueous sodium carbonate solution, and then 369 mg (0.32 mmol) of tetrakis (triphenyl phosphine)palladium (0) were added and heated under reflux for 7 hours. After completion of the reaction, ethyl acetate and water were added to the reaction mixture. The organic layer was separated, washed with a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. Filtration was then carried out, and the filtrate was condensed. The resulting crude product was separated and purified using silica gel column chromatography to give N-(3'-amino-4'-methylbiphenyl-4-yl)acetamido (yield: 66%). 1H-NMR (CDCl3) delta: 2.19 (3H, s), 2.20 (3H, s), 3.68 (2H, br), 6.88-6.94 (2H, m), 7.10 (1H, d, J = 7.4 Hz), 7.29-7.32 (1H, m), 7.48-7.55 (4H, m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
74% | With sodium carbonate;tetrakis(triphenylphosphine) palladium(0); In 1,2-dimethoxyethane; water; for 7h;Reflux; | (i) N-(3'-amino-4'-methylbiphenyl-3-yl)acetamido; 0.67 g (3.61 mmol) of 5-bromo-2-methylaniline and 1.14 g (4.37 mmol) of <strong>[480424-93-9]3-acetamidophenyl boronic acid pinacol ester</strong> were dissolved in 15 mL of DME. Subsequently, 5 mL of a 2M aqueous sodium carbonate solution, and then 417 mg (0.36 mmol) of tetrakis(triphenyl phosphine)palladium (0) were added to the mixture, and the mixture was heated under reflux for 7 hours. After completion of the reaction, ethyl acetate and water were added to the reaction mixture. The organic layer was separated, washed with a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. Filtration was conducted, and the filtrate was condensed. The resulting crude product was separated and purified using silica gel column chromatography to give N-(3'-amino-4'-methylbiphenyl-3-yl)acetamido (yield: 74%). 1H-NMR (CDCl3) delta: 2.19 (3H, s), 2.20 (3H, s), 3.68 (2H, br), 6.88-6.94 (2H, m), 7.10 (1H, d, J = 7.4 Hz), 7.30-7.69 (5H, m). |
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