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CAS No. : | 2142-69-0 | MDL No. : | MFCD00000067 |
Formula : | C8H7BrO | Boiling Point : | - |
Linear Structure Formula : | BrC6H4C(O)CH3 | InChI Key : | PIMNFNXBTGPCIL-UHFFFAOYSA-N |
M.W : | 199.04 | Pubchem ID : | 75060 |
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 |
---|---|---|
100% | With pyridine; selenium(IV) oxide; at 100℃; for 2h; | 8.3 g (75 mmoles) of selenium dioxide were added to 10 g (50 mmoles) of 2'- bromoacetophenone dissolved in 20 ml of pyridine; the mixture was left under magnetic stirring at 100C for 2 hours. After control in TLC and LC-MS, the mixture was filtered to eliminate the selenium and the pyridine was removed at reduced pressure. The residue was acidified with diluted HCl and extracted with ethyl acetate; the phases were then separated; the aqueous phase was re- extracted twice with ethyl acetate. The organic phases were joined and washed with water and a saturated solution of NaCl. After anhydrification on sodium sulfate, filtration and evaporation of the solvent at reduced pressure, 11.4 g of the desired product (50 mmoles) were obtained, as a cream-coloured solid. The raw product thus obtained was used for the subsequent reaction. Quantitative yield. LC-MS [M+H] = 229. |
87% | With pyridine; selenium(IV) oxide; at 120℃; for 18h;Inert atmosphere; | Into a 250-mL 3-necked round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of l-(2-bromophenyl)ethan-l-one (10 g, 50.24 mmol, 1.00 equiv) in pyridine (80 mL). This was followed by the addition of Se02 (22 g, 198.27 mmol, 3.95 equiv). The resulting solution was stirred for 18 h at 120 C in an oil bath. The reaction mixture was cooled to room temperature. The solids were filtered out. The resulting mixture was concentrated under vacuum. The residue was dissolved in 100 mL of water. The resulting mixture was washed with 2x50 mL of ethyl acetate. The pH value of the aqueous layer was adjusted to 1-2 with hydrogen chloride (4 mol/L). The resulting solution was extracted with 3x80 mL of ethyl acetate and the organic layers combined and dried over anhydrous sodium sulfate. The solids were filtered out. The resulting mixture was concentrated under vacuum. This resulted in 10 g (87%) of 2-(2- bromophenyl)-2-oxoacetic acid as yellow oil. MS (ESI) m/z 230 ([M + H]+) |
With pyridine; selenium(IV) oxide; at 90 - 110℃; for 5h; | General procedure: The substituted alpha-keto acids were prepared from oxidation of corresponding methyl ketones with SeO2 (Scheme 1). Methyl ketones (5 mmol), SeO2 (6 mmol), 20 mL of pyridine were added in a 50 mL round-bottom flask. The reaction mixture was stirred at 110 oC for 1 h, and under 90 oC for another 4 h. The desired products were isolated by silica-gel column chromatography. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
69.3% | In ethanol;Reflux; | General procedure: solutionof acid hydrazide (0.01 mol) and appropriate benzaldehyde/acetophenone (0.01 mol) in ethanol was refluxed for 5-6 h. The precipitated title compounds were then filtered off, washed with water and recrystallized from ethanol. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
54% | O-bromoacetophenone 1a (119.4 mg, 0.12 mmol) was sequentially added to a 25 mL round bottom flask as described in Example 1,0.6 mmol), dimethylsulfoxide (3 mL) and iodine (152 mg, 0.6 mmol) were added and the mixture was stirred under heating at 110 ° C for 3 h, then cooledBut to room temperature, 2d (68.2 mg, 0.4 mmol), CuBr (11.5 mg, 0.08 mmol) and K2CO3 (221 mg, 1.6 mmol)The reaction was stirred at room temperature for 5h, then heated and stirred at 100 for 3h. After the reaction was completed, saturated chlorination was added to the reaction vesselThe reaction was quenched with ammonium chloride and extracted with dichloromethane. The combined organic phases were washed with deionized water and saturated sodium chloride solution,Sodium drying. Filtration, spin-drying, separation through a silica gel column (petroleum ether / ethyl acetate = 2/1, v / v)3-Chloroindole [2,1-b] quinazoline-6,12-dione 3k (61 mg, 54percent). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | In ethanol; at 20℃; for 16h; | A solution of 2-bromoacetophenone (1.99 g, 10 mmol) and tert-butyl (2-amino 2-thioxoethyl)carbamate (1.90 g, 10 mmol) in EtOH (50 mL) was stirred at room temperature for 16 h. The solution was evaporated and the resulting residue diluted in water (25 mL) and extracted with EtOAc (2 x 25 mL). The combined extracts were dried and evaporated affording a pale yellow solid. Recrystallisation from MeCN (13 mL) led to colourless solid (2.03 g, 70%). M/z 235 (M+H-tBu)+. |
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