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CAS No. : | 89180-45-0 | MDL No. : | MFCD11109884 |
Formula : | C4H3ClN2O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MPQIKXKJHKXJQC-UHFFFAOYSA-N |
M.W : | 130.53 | Pubchem ID : | 14774300 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338-P310 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-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 120℃; for 2h; | A mixture of 2-hydroxy-5-chloropyrazine in POCl3 (21 equiv.) was heated at 1200C for 2 h. The reaction mixture was cooled and poured on ice and extracted with dichloromethane. The organic solvent was collected, dried over Na2SO4 and filtered. The solvent was filtered over silica gel followed by ethyl acetate. The solvents were evaporated to provide the title compound | |
With trichlorophosphate; at 130℃; for 6h; | [Referential Example 11] 1-(5-Methoxy-2-pyrazinyl)-5-(2-pyridyl)-1H-pyrazole-3-carboxylic acid; [Show Image] [Show Image] 1) 5-Chloro-2-hydrazinopyrazine; A solution of 5-chloro-2-hydroxpyrazine (1.84 g) synthesized from aminopyrazine by the method of Palamidessi et al. (J.Org.Chem., vol.29, pp 2491-2492, 1964) in phosphorus oxychloride (28ml) was placed in a sealed tube, and the solution was stirred at an outer temperature of 130°C for 6 hours. After cooling with air, ice cold water and dichloromethane were added to the reaction liquid, then the phases were separated. The organic layer was dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure. Hydrazine monohydrate (1.39 ml) was added to a solution of the residue in ethanol (14 ml), and the mixture was stirred at room temperature for 150 minutes and for another 15 minutes at 80°C. After cooling with air, the reaction liquid was evaporated under reduced pressure, and to the residue was added water and a mixed solvent of chloroform and methanol (1:10), then the phases were separated. The organic layer was dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure to give 5-chloro-2-hydrazinopyrazine(0.325 g, 16percent) as a solid. 1H-NMR (400 MHz, DMSO-d6)delta: 4.32 (2H, br s), 7.92 (1H, s), 7.99 (1H, s), 8.13 (1H, s). EI-MSm/z: 144 (M+). |
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