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CAS No. : | 74420-02-3 | MDL No. : | MFCD08272229 |
Formula : | C7H6N2O | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | IXIGMDXJXKDZOF-UHFFFAOYSA-N |
M.W : | 134.14 | Pubchem ID : | 12646048 |
Synonyms : |
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Chemical Name : | 4-Hydroxy-7-azaindole |
Signal Word: | Warning | Class: | |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302 | Packing Group: | |
GHS Pictogram: |
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* 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 |
---|---|---|
21% | With caesium carbonate; In N,N-dimethyl-formamide; at 20 - 60℃; for 8.5h; | To a solution of compound lH-pyrrolo[2,3-]pyridin-4-ol (0.1 mmol, 13.4 mg, prepared generally according to the procedures outlined by Thibault, C. et al.Org. Lett. 2003, 5, 5023-5025, the disclosure of which is incorporated by reference, in DMF (1 mL) was added cesium carbonate (Aldrich, 0.25 mmol, 81 mg). The mixture was stirred at room temperature for 0.5 h. To this mixture was added 2,4,5-trifluoro- iV-(l-(4-fluorophenyl)-2-oxo-l,2-dihydropyridin-3-yl)beiizamide (36 mg, 0.1 mmol). The reaction mixture was heated at 60 0C for 8 h. After the reaction mixture was cooled to room temperature, 2 mL of cold water was added. The reaction mixture was extracted with EtOAc (3 x 20 mL). The organic extracts were dried with MgSO4, concentrated in vacuo, and purified by preparative HPLC. The desired fractions were combined, concentrated in vacuo, and lyophilized to dry to give the title compound (trifluoroacetic acid salt, 10.0 mg, 21percent yield) as a white solid. 1H NMR (CD3OD) delta 8.61 (d, IH, J= 5.7 Hz), 8.26 (d, IH, J= 6.6 Hz), 8.02 (dd, IH, J= 11.0, 6.6 Hz), 7.51 (d, IH, J= 3.9 Hz), 7.29-7.25 (m, 3H), 7.36 (d, IH, J= 6.6 Hz), 7.25 (t, 2H, J= 8.8 Hz), 6.90 (d, IH, J= 6.6 Hz), 6.60 (d, IH, J= 3.3 Hz), 6.50 (t, IH, J= 7.2 Hz); MS(ESI+) m/z All..22 (M + H)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | With triphenylphosphine; diethylazodicarboxylate; In tetrahydrofuran; at 20℃;Inert atmosphere; | 4-Ethoxy-1H-pyrrolo[2,3-b]pyridineDiethyl azodicarboxylate (DEAD) (520 mul, 3.3 mmol) is added dropwise, at ambient temperature and under an inert atmosphere, to a solution of PPh3 (1.04 g, 3.96 mmol) in anhydrous THF (13 ml). This solution is transferred via a tube, under an inert atmosphere, into a round-bottomed flask containing a solution of <strong>[74420-02-3]4-hydroxy-7-azaindole</strong> (222 mg, 1.65 mmol) and ethanol (115 mul, 1.98 mmol) in anhydrous tetrahydrofuran (THE) (41 ml). The solution is stirred at ambient temperature for 2 h. The solvent is evaporated. The residue obtained is purified with a chromatography column (eluent: CH2Cl2/MeOH 98:2) to give the desired compound (214 mg, 80percent). Solid; M.p.=176-178° C. (Et2O); 1H NMR (300 MHz, CDCl3) delta 1.52 (t, 3H, J=7.1 Hz, CH3), 4.26 (q, 2H, J=7.1 Hz, CH2), 6.53 (d, 1H, J=5.6 Hz, Harom), 6.59 (broad s, 1H, Harom), 7.18 (broad s, 1H, Harom), 8.18 (d, 1H, J=5.6 Hz, Harom), 9.64 (broad s, 1H, NH); MS (SI) m/z 163 (M+H+). |
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