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CAS No. : | 26218-78-0 | MDL No. : | MFCD04972371 |
Formula : | C7H6BrNO2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | NFLROFLPSNZIAH-UHFFFAOYSA-N |
M.W : | 216.03 | Pubchem ID : | 13349623 |
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 |
---|---|---|
10% | With 3,3-dimethyl-butan-2-one; palladium diacetate; potassium carbonate; tri tert-butylphosphoniumtetrafluoroborate; In N,N-dimethyl-formamide; at 110℃; for 6.0h;Inert atmosphere; | j0235] Procedure:10236] Pd(OAc)2 (15.7 mg, 0.070 mmoles), [P(t-13u)3H] HF4 (60.7 mg, 0.21 mmoles), pivalic acid (28.5 mg, 0.28 mmoles), K2C03 (386 mg, 2.8 mmoles), methyl thiazole-4- carboxylate (200 mg, 1.4 mmoles), and methyl 6-bromoni- cotinate (603 mg, 2.8 mmoles) were added to a dried flask. The flask was fitted with a reflux condenser capped with a septum, evacuated, and purged with nitrogen (.-5 times). Dry DMF (7 mE) was added via syringe, and the reaction was stirred at 1100 C. for 6 h. The reaction mixture was cooled and filtered through Celite, and the filtrate was concentrated under reduced pressure. The crude product was then purified by chromatography on silica (1% acetone in DCM) to afford the title compound (39 mg, 10%) as a white solid. ?H NMR (400 MHz, CDC13) oe 9.18 (dd, J=0.8, 2.0 Hz, 1H), 8.41 (dd, J=2.0, 8.4 Hz, 1H), 8.38 (dd, J=0.8, 8.4 Hz, 1H),8.33 (s, 1H), 3.99 (s, 3H), 3.98 (s, 3H); ?3C NMR (100 MHz, CDC13) oe 168.7, 165.1, 161.7, 153.3, 150.7, 148.3, 138.3, 130.7, 126.9, 119.6, 52.6, 52.6; HRMS (ESI) mlz 279.0423 [calc?d for C,2H,,N204S (M+H) 279.0435]. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
29% | With 1-Adamantanecarboxylic acid; palladium diacetate; potassium carbonate; tri tert-butylphosphoniumtetrafluoroborate; In toluene; at 110℃; for 8h;Inert atmosphere; | j0238] Procedure:10239] Pd(OAc)2 (31.8 mg, 0.14 mmoles), [P(t-13u)3H] HF4 (123.2 mg, 0.42 mmoles), 1-adamantanecarboxylic acid (153 mg, 0.85 mmoles), K2C03 (782 mg, 5.7 mmoles), and methyl 6-bromonicotinate (918mg, 4.3 mmoles) were added to a dried flask. The flask was fitted with a reflux condenser capped with a septum, evacuated, and purged with nitrogen (.-5 times). A degassed solution of ethyl oxazole-5-carboxy- late (400 mg, 2.8 mmoles) in dry toluene (7 mE) was added via syringe, and the reaction was stirred at 1100 C. for 8 h. The reaction mixture was cooled and filtered through Celite, and the filtrate was concentrated under reduced pressure. The crude product was then purified by chromatography on silica (30% EtOAc in hexanes followed by 2% acetone in 1:1 DCM:hexanes) to afford the title compound (183 mg, 23%) as a white solid. ?H NMR (400 MHz, CDC13) oe 9.37 (dd, J=0.8, 2.0 Hz, 1H), 8.47 (dd, J=2.0, 8.0 Hz, 1H), 8.30 (dd, J=0.8, 8 Hz, 1H), 7.96 (s, 1H), 4.46 (q, J=7.2 Hz, 2H), 4.00 (s, 3H), 1.43 (t, J=7.2 Hz, 3H); ?3C NMR (100 MHz, CDC13) oe 164.9, 161.6, 157.5, 151.5, 148.0, 143.8, 138.3, 135.5, 127.3, 122.5, 61.9, 52.7, 14.3; HRMS (ESI) mlz 277.0823 [calc?d for C,3H,3N205 (M+H) 279.0819]. For experiments with mammalian cells, this compound was recrystallized from EtOAc to afford a white crystalline solid |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
29% | With 3,3-dimethyl-butan-2-one; palladium diacetate; potassium carbonate; tri tert-butylphosphoniumtetrafluoroborate; In toluene; at 110℃; for 24h;Inert atmosphere; | j0241] Procedure:j0242] Pd(OAc)2 (15.9 mg, 0.071 mmoles), [P(t-Hu)3H] HF4 (61.8 mg, 0.21 mmoles), pivalic acid (29.0 mg, 0.28 mmoles), K2C03 (391 mg, 2.8 mmoles), ethyl oxazole-4- carboxylate (200 mg, 1.4 mmoles), and methyl 6-bromoni- cotinate (612 mg, 2.8 mmoles) were added to a dried flask. The flask was fitted with a reflux condenser capped with a septum, evacuated, and purged with nitrogen (.-5 times). Drytoluene (7 mE) was added via syringe, and the reaction was stirred at 1100 C. for 24 h. The reaction mixture was cooled and filtered through Celite, and the filtrate was concentrated under reduced pressure. The crude product was then purified via chromatography on silica (2% acetone in DCM followed by 10% acetone 1:1 DCM:hexanes) to afford the title compound (113 mg, 29%) as a white solid. ?H NMR (400 MHz, CDC13) oe 9.31 (dd, J=0.8, 2.0 Hz, 1H), 8.46 (dd, J=2.0, 8.4 Hz, 1H), 8.42 (s, 1H), 8.38 (dd, J=0.8, 8.4 Hz, 1H), 4.45 (q, J=7.2 Hz, 2H), 4.00 (s, 3H), 1.42 (t, J=7.2 Hz, 3H); ?3C NMR (100 MHz, CDC13) oe 164.9, 160.8, 160.2,151.1, 148.0, 145.2, 138.3, 135.3, 127.1, 122.3, 61.6, 52.7, 14.3; HRMS (ESI) mlz 277.0815 [calc?d for C,3H,3N205 (M+H) 277.0823]. |
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