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CAS No. : | 60186-16-5 | MDL No. : | MFCD06659522 |
Formula : | C5H2ClFN2O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | QYRFYYRMUFOIKW-UHFFFAOYSA-N |
M.W : | 176.53 | Pubchem ID : | 12275768 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-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 |
---|---|---|
aluminum nickel; In ethanol; hexane; ethyl acetate; | Example P10 3-Amino-5-chloro-2-fluoropyridine 7.5 g (0.042 mol) of <strong>[60186-16-5]5-chloro-2-fluoro-3-nitropyridine</strong> are dissolved in 80 ml of ethanol. This solution is hydrogenated with hydrogen, in the presence of 1 g of Raney nickel catalyst, under normal pressure and at a temperature in the range from 20 to 25 C. After a hydrogenation period of 20 hours, the catalyst is removed and the solvent is evaporated off. The residue is taken up in ethyl acetate and the resultant solution is filtered through a layer of silica gel. The solvent is evaporated off and the residue is triturated in hexane. The precipitate is subsequently filtered and dried, affording 4.7 g (76%) of 3-amino-5-chloro-2-fluoropyridine, m.p. 74 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In tetrahydrofuran; at 0 - 20℃; for 6.16667h;Reflux; | 4-(5-Chloro-3-nitropyridin-2-yl)morpholine To a stirred solution of <strong>[60186-16-5]5-chloro-2-fluoro-3-nitropyridine</strong> (5 g, 28 mmol) in THF (40 mL) was added morpholine (4 mL, 42 mmol). The reaction was stirred at 0 C. for ten min, at rt for 1 h, and refluxed for four h. The reaction was then cooled to rt, taken up in EtOAc, and washed with satd aq. sodium bicarbonate and brine. The organic layer was dried (magnesium sulfate) and concentrated, affording 4-(5-chloro-3-nitropyridin-2-yl)morpholine as a yellow oil. Mass Spectrum (ESI) m/e=244.0 (M+1). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
520 mg | With 1-methyl-pyrrolidin-2-one; N-ethyl-N,N-diisopropylamine; In acetonitrile; for 3.0h;Reflux; | General procedure: A mixture of 2-chloro-4-phenylpyrimidine (71 mg, 0.37 mmol), Intermediate 20 (100 mg, 0.34 mmol) and DIPEA (120 muIota_, 0.68 mmol) in NMP (1 mL) was heated at 130C for 3 hrs. The reaction mixture was allowed to cool to ambient temperature and diluted with water (10 mL). The crude product was extracted into diethyl ether (20 mL), dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by chromatography on the Biotage Companion (12 g column, 0 to 100% diethyl ether in isohexane) to afford the title compound as a gum (65 mg). LCMS (Method A): Two peaks at 2.45 min and 2.66 min, 451 [M+H]+.1H NMR (400 MHz, DMSO-d6, 374 K) 8.36 (d, 0.8 H), 8.30 (bd, 0.2 H), 8.15-8.07 (m, 1 .6 H), 7.97 (bm, 0.3 H), 7.56-7.46 (m, 3.92 H), 7.46-7.24 (m, 7.38 H), 7.16-7.05 (m, 1.8 H), 6.33 (bs, 1 H), 4.41 (td, 1 H), 3.71 (m, 1 H), 3.50 (m, 1 .1 H), 3.26 (bm, 0.2 H), 2.84 (s, 0.3 H), 2.82 (s, 0.3 H), 2.63 (s, 0.3 H), 2.48 (s, 2.1 H), 1 .82 (bm, 0.7 H), 1.00 (d, 2.5 H), 0.78 (bd, 0.5 H), 0.56 (bs, 3 H). |
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