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CAS No. : | 1168102-35-9 | MDL No. : | MFCD20482789 |
Formula : | C8H5ClN2O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 196.59 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Class: | ||
Precautionary Statements: | UN#: | ||
Hazard Statements: | Packing Group: |
* 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 |
---|---|---|
43% | tetrakis(triphenylphosphine) palladium(0); In N,N-dimethyl-formamide; at 190℃; for 0.333333h;microwave irradiation; | 3-Chloro-2-cvano-isonicotinic acid methyl ester <n="48"/>[00199] A microwave vial was charged with 2,3-dichloro-isonicotinic acid methyl ester(7.6 g, 36.9 mmol), zinc cyanide (4.75 g, 40.6 mmol), tetrakis(triphenylphosphine)palladium (1.0 g, 0.9 mmol) and DMF (37 mL), then capped, evacuated and backfilled with nitrogen. The reaction solution was subjected to microwave irradiation, heating at 1900C for 20 minutes, then filtered through a pad of Celite which was washed further with ethyl acetate. The resulting mixture was washed with water, followed by a saturated solution of sodium hydrogen carbonate, then brine, dried (Na2SO4), filtered and concentrated in vacuo. The resultant residue was subjected to column chromatography (Si-PPC, gradient 0% to 100%, ethyl acetate in cyclohexane) to give the title compound as a white solid (3.1 g, 43%). 1H NMR (CDCI3, 400MHz) 8.70 (d, J=5.0 Hz, IH), 7.87 (d, J=5.0 Hz, IH), 4.01 (s, 3H). |