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CAS No. : | 24782-43-2 | MDL No. : | MFCD01863732 |
Formula : | C12H11NO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | UACLREXZGKWWIC-UHFFFAOYSA-N |
M.W : | 217.22 | Pubchem ID : | 282844 |
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 |
---|---|---|
With trichlorophosphate; at 100℃; for 0.5h;Microwave irradiation; | Intermediate 10; Ethyl 4-chloroquinoline-2-carboxylatePhosphorous oxychloride (5ml) was added to <strong>[24782-43-2]ethyl 4-hydroxyquinoline-2-carboxylate</strong> (l.Olg). The reaction mixture was subjected to single-mode microwave at 100 0C for 30 min using a Smith Microwave Synthesizer. The solvent was removed in vacuo and recrystallized with acetone to gave the title compound as a white solid (1.9Og). MS (ES) MH+: 235, 237 for C12Hi0ClNO2; NMR (CDCl3): 1.44 (t, 3H, J = 7.16), 4.51 (q, 2H, J = 7.16), 7.19 (s, IH), 7.71 (m, IH), 7.81 (m, IH), 8.22 (m, IH), 8.36 (d, IH, J = 8.29). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With phosphorus(V) oxybromide; In toluene; acetonitrile; at 75℃; for 1.5h; | EXAMPLE 14-[(6-Chloropyridin-3-yl)methyl]-N-[(i5,2^-2-hydroxycyclohexyl]quinoline-2--carboxairiideA solution of <strong>[24782-43-2]ethyl 4-hydroxyquinoline-2-carboxylate</strong> (10.0 g, 46.0 mmol) and phosphorus oxybromide (13.2 g, 46.0 mmol) in 100 mL of toluene and 10.0 mL acetonitrile was heated at 75 C for 1.5 h. The reaction mixture was cooled to room temperature, quenched slowly with water, and extracted with ethyl acetate. The organic fraction was washed with brine, dried over sodium sulfate, filtered, and concentrated. The resultant residue was subjected to silica gelchromatography eluting with 0-50% ethyl acetate in hexanes to afford ethyl 4-bromoquinoline-2~ carboxylate that gave a mass ion (ES+) of 280.1 (79Br) for M+H+. | |
With phosphorus(V) oxybromide; In toluene; acetonitrile; at 75℃; for 1.5h; | solution of <strong>[24782-43-2]ethyl 4-hydroxyquinoline-2-carboxylate</strong> (10.0 g, 46.0 mmol) and phosphorus oxybromide (13.2 g,46.0 mmol) in 100 mL of toluene and 10.0 mL acetonitrile was heated at 75 C for 1.5 h. The reaction mixture was cooledto room temperature, quenched slowly with water, and extracted with ethyl acetate. The organic fraction was washedwith brine, dried over sodium sulfate, filtered, and concentrated. The resultant residue was subjected to silica gel chromatographyeluting with 0-50% ethyl acetate in hexanes to afford ethyl 4-bromoquinoline-2-carboxylate that gave a massion (ES+) of 280.1 (79Br) for M+H+. |
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