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CAS No. : | 85290-78-4 | MDL No. : | MFCD00233457 |
Formula : | C7H10N2O2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | HHYVTIKYZUMDIL-UHFFFAOYSA-N |
M.W : | 154.17 | Pubchem ID : | 227598 |
Synonyms : |
|
Chemical Name : | Ethyl 3-methyl-1H-pyrazole-4-carboxylate |
Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
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 |
---|---|---|
73% | With sodium hydride; In N,N-dimethyl-formamide; at 180℃; | A mixture of <strong>[85290-78-4]ethyl 3-methyl-1H-pyrazole-4-carboxylate</strong> (7.95 g), 2-chloropyridine (5 ml), sodium hydride (60%, oil, 2.32 g) and N,N-dimethylformamide (150 ml) was stirred overnight at 180 DEG C. The reaction mixture was poured into water and extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to give ethyl 3-methyl-1-(2-pyridyl)-1H-pyrazole-4-carboxylate (8.31 g, yield 73%) as colorless crystals from a fraction eluted with ethyl acetate-hexane (1:9, volume ratio). The crystals were recrystallized from ethyl acetate-hexane. melting point: 79-80 DEG C. |
73% | With sodium hydride; In DMF (N,N-dimethyl-formamide); at 180℃; | A mixture of <strong>[85290-78-4]ethyl 3-methyl-1H-pyrazole-4-carboxylate</strong> (7.59 g), 2-chloropyridine (5 ml), sodium hydride (60%, oily, 2.32 g) and N,N-dimethylformamide (150 ml) was stirred at 180C overnight. The reaction mixture was poured into water, which was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution, dried (MgSO4) and concentrated. The residue was subjected to silica gel column chromatography to obtain ethyl 3-methyl-1-(2-pyridyl)-1H-pyrazole-4-carboxylate (8.31 g, yield 73%) from the fraction eluted with ethyl acetate-hexane (1:9, volume ratio). This was recrystallized from ethyl acetate-hexane. Melting point: 79-80C |
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