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CAS No. : | 65340-70-7 | MDL No. : | MFCD00511001 |
Formula : | C9H5BrClN | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | KJILYZMXTLCPDQ-UHFFFAOYSA-N |
M.W : | 242.50 | Pubchem ID : | 5139537 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P264-P271-P280-P305+P351+P338-P302+P352-P304+P340-P312-P362+P364-P403+P233-P501 | 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 |
---|---|---|
With triethylamine; In DMF (N,N-dimethyl-formamide); at 130℃; for 8h; | Production Example 82 1-(6-Bromo-4-quinolyl)-4-piperidyl methyl ether A mixture of 500 mg 6-bromo-4-chloroquinoline, 330 mg <strong>[4045-25-4]4-methoxypiperidine monohydrochloride</strong>, 0.57 ML triethylamine and 10 ML N,N-dimethylformamide was stirred at 130C for 8 hours.. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated.. The organic layer was washed with water and brine and dried over sodium sulfate, and the solvent was evaporated.. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 516mg of the title compound as a pale yellow oil.1H-NMR (CDCl3) delta: 1.85-1.98(m, 2H), 2.08-2.20(m, 2H), 2.97-3.08(m, 2H), 3.38-3.55(m, 6H), 6.85(d, J=5.0Hz, 1H), 7.70(d, J=8.6Hz, 1H), 7.90(d, J=8.6Hz, 1H), 8.12(s, 1H), 8.69(d, J=5.0Hz, 1H) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90.8% | In methanol; at 20 - 120℃; for 15h; | To a solution of 6-bromo-4-chloro-quinoline (12.12 g, 50 mmol) in methanol (200 mL) was added sodium methoxide (13.50 g, 250 mmol) at room temperature. Then, the reaction mixture was heated to 120 C. for 15 h in a sealed reaction flask. After cooling to room temperature, the methanol was removed under the vacuum and the residue was diluted with water. Then, the solids were collected by filtration and washed with water. After drying in air, 10.8 g (90.8% yield) of 6-bromo-4-methoxy-quinoline was isolated as a white solid which can be crystallized from acetonitrile: EI-HRMS m/e calcd for C10H8BrNO (M+) 236.9789, found 236.9784. |
36% | In methanol; at 120℃; for 1h;Microwave irradiation; | 300 mg (1.24 mmol) of 6-bromo-4-chloroquinoline [Lin et al., J. Med. Chem. 1978, 21, 268] was taken up in 4 ml methanol and 1.15 ml (6.19 mmol) methanolic sodium methylate solution (30 wt.%) was added. Then it was reacted in a single mode microwave for 1 h at 1200C. The solvent was removed in a rotary evaporator and the residue was partitioned between water and ethyl acetate. The aqueous phase was extracted with ethyl acetate and the combined organic phases were dried over magnesium sulfate. The solvent was removed by distillation at reduced pressure. In this way we obtained 150 mg (36% of theor.) of the target compound.LC-MS (method 2): R, = 1.24 min; MS (EIpos): m/z = 238 [M]+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
at 100℃; for 1h; | A 5 mL microwave vial was charged with 4-chloro-6-bromoquinoline (0.15 g, 0.62 mmol) and a 25 wt % solution of sodium methoxide in methanol (2.0 mL, 8.8 mmol). The vial was sealed and heated to 100C for 60 minutes under microwave irradiation (Biotage, Initiator). After cooling, the solvent was removed in vacuo, the residue washed with water, filtered and dried via .yophilization to obtain 6-bromo-4-methoxyquinoline.LRMS (ESI) calc'd for C10H9BrNO [M+H]+: 238, Found: 238. |
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