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CAS No. : | 5424-43-1 | MDL No. : | MFCD00185638 |
Formula : | C8H9BrO2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | UCEJNFOIRGNMKV-UHFFFAOYSA-N |
M.W : | 217.06 | Pubchem ID : | 224013 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | 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 |
---|---|---|
73% | With aluminum (III) chloride; In toluene; for 3h;Heating / reflux; | To 2,3-dimethoxy-bromobenzene (8.2 g, 0.45 moles) in 50 ML of toluene was added AlCl3 (22.1 g, 0.178 moles).. The reaction mixture was refluxed for 3 hours, cooled, poured into 800 ML of water, and extracted with 800 ML of ether.. The ether extracts were dried over magnesium sulfate, filter and the solvent removed under reduced pressure.. The residue was chromatographed on silica gel, eluted with methylene chloride and the fraction were combined and evaporated under reduced pressure to yield 2,3-dihydroxy-bromobenzene (6.1 g, 73percent yield). |
The l-bromo-2,3-dimethoxybenzene (2.17 g, 10 mmol) was dissolved in DCM (60 ml) and treated with 1.0 M DCM solution OfBBr3 (15 mL, 15 mmol) at 0 °C and then allowed to warm to room temperature. After stirring overnight, the reaction mixture was cooled to 0 0C, 2 mL of MeOH was added, and the solvent was removed under vacuum. The residue was dissolved in 20 mL of EtOAc and washed with IN HCl (2 x 50 mL), water, brine and dried over Na2SO4. The solvent was removed under vacuum. The crude residue was then dissolved in DMF (40 mL) and Cs2CO3 (9.75 g, 30 mmol) and 2- (benzyloxycarbonylamino)ethyl methanesulfonate (6.8 g, 25 mmol) were added. After stirring at 100 0C under nitrogen for 2 h, a further amount OfCs2CO3 (9.75 g, 30 mmol) and 2-(benzyloxycarbonylamino)ethyl methanesulfonate (6.8 g, 25 mmol) were added. After stirring at 100 0C for 2 h, the reaction mixture was poured onto water (900 mL) and extracted with EtOAc (3 x 100 mL). The organic layers were combined, washed with water (50 mL) and dried over Na2SO4. The solvent was removed under vacuum and purified by flash chromatography using cyclohexane/EtOAc (8/2) as eluent to afford the title compound (2.45 g, 45percent yield) as a white solid. <n="54"/>ESMS; m/z 543, 545 (M+l), 560, 562 (M+18)1H-NMR (CDCl3): 63.54 (m, 4H), 4.06 (m, 4H), 5.09 (s, 4H), 5.62(bs, IH), 5.75(bs, IH), 6.82 (d, J= 8 Hz, IH), 6.91 (t, J= 8 Hz, IH), 7.13 (dd, J= 8 Hz, J= 1.3 Hz, IH), 7.32 (m, 10H). 13C-NMR (CDCl3): 540.5, 41.3, 66.8, 68.2, 71.8, 112.9, 118.0, 125.4, 128.1, 128.2, 128.5, 136.4, 152.6, 156.5.Theoretical Mass: (M + Na) 565.09501. Measured Mass: (M + Na) 565.09508 Microanalysis: percentC 57.58 (57.47), percentH 5.10 (5.01), percentN 5.16 (5.04) M.p. 54°C |
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