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CAS No. : | 943-14-6 | MDL No. : | MFCD00134558 |
Formula : | C7H4BrNO4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 246.02 | Pubchem ID : | - |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | 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 |
---|---|---|
81% | for 12 h; Heating / reflux | 2-Bromo-5-nitro benzoic acid methyl ester was prepared according to the Reaction Formula 4 shown below: (yield: 81percent): White Crystal1H NMR (400 MHz, CDCl3)=4.00 (s, 3H), 7.88 (d, J=8.76 Hz, 1H), 8.18 (dd, J=2.76 Hz and 2.76 Hz, 1H), 8.66 (d, J=2.74 Hz, 1H) 13C NMR (100 MHz, CDCl3)=53.12, 126.33, 126.61, 129.24, 133.12, 135.71, 146.70, 164.48 |
79% | at 0℃; for 2 h; Reflux | 2-bromo-5-nitrobenzoic acid (1.96 g, 7.96 mmol) was dissolved in methanol (20 mL) and cooled to 0 °C. Thionyl chloride (1.60 mL, 23.9 mmol) was added dropwise to the solution. The reaction mixture was then refluxed for 2 hrs. The mixture was evaporated under reduced pressure to a solid which was then taken up in 100 mL of ethyl acetate. The solution was washed with 2x 100 mL of water. The organic layer was dried with magnesium sulfate and filtered. The solution was evaporated under reduced pressure to yield a yellow solid (1.63 g, 79percent). mp = 78-80 °C. 1H NMR (400 MHz, CDCl3): δ 8.66 (d, J = 2.8 Hz, 1 H), 8.16 (dd, J = 8.8, 2.8 Hz, 1 H), 7.87 (d, J = 8.8 Hz, 1 H), 4.00 (s, 3 H). 13C NMR (100 MHz, CDCl3): δ 164.5, 147.3, 145.5, 135.7, 133.2, 129.3, 126.6, 126.4, 53.1. FT-IR (thin film, cm-1): 1740.94, 1531.97, 1348.35. TOF-MS (ESI, [M+H]+) calculated for C8H7NO4Br 259.9553; found 259.9502. |
2.83 g | With sulfuric acid In dichloromethane at 20℃; for 3 h; Reflux | Example 21: preparation of intermediate 21: methyl 2-bromo-5-nitrobenzoate2-bromo-5-nitrobenzoic acid (4g, 0.Ol6mol) was dissolved in MeOH (20m1) and sulphuric acid (imI) was added. The reaction was refluxed for 3h then cooled at RT. Water (20m1) was added and the solid was filtered, dissolved in DCM andwashed with saturated aqueous solution of NaHCO3. The organic solvent wasdried (Na2504) and evaporated. Intermediate 21 was obtained as white solid(2.83g). |
2.83 g | for 3 h; Reflux | 2-bromo-5-nitrobenzoic acid (4 g, 0.016 mol) was dissolved in MeOH (20 ml) and sulphuric acid (1 ml) was added. The reaction was refluxed for 3 h then cooled at RT. Water (20 ml) was added and the solid was filtered, dissolved in DCM and washed with saturated aqueous solution of NaHCO3. The organic solvent was dried (Na2SO4) and evaporated. Intermediate 21 was obtained as white solid (2.83 g). [0256] MS (ESI) m/z: 231 [M+H]+. [0257] 1HNMR (CDCl3) δ ppm=8.67 (d, 1H), 8.18 (dd, 1H), 7.90 (d, 1H), 4.02 (s, 3H) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1 g | Stage #1: With oxalyl dichloride In dichloromethane at 20℃; for 0.5 h; Stage #2: at 20℃; for 2 h; |
To a solution of 2-bromo-5-nitrobenzoic acid (1.50 g, 6.12 mmol) in CH2CI2 (10 mL) was added oxalyl chloride (1.10 g, 12.24 mmol) and the resulting solution was stirred at rt for 30 minutes. Then the reaction mixture was concentrated and the residue was dissolved in EtOH and the resulting solution was stirred at rt for 2h before it was concentrated and the residue was dissolved in EtOAc. Then water was added to the resulting solution and the organic layer was washed with brine, separated, dried, filtered and concentrated to afford 1.0 g of the title product. 1H NMR (300 MHz, DMSO-i): δ 8.50 (d, J = 3.0 Hz, 1H), 8.27-8.23 (dd, J = 3.0, 8.7 Hz, 1H), 8.06-8.03 (d, J = 8.7 Hz, 1H), 4.41-4.34 (q, J = 6.9 Hz, 2H), 1.37-1.32 (t, J = 7.2 Hz, 3H). |
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