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CAS No. : | 23056-36-2 | MDL No. : | MFCD00661454 |
Formula : | C5H3ClN2O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | LIEPVGBDUYKPLC-UHFFFAOYSA-N |
M.W : | 158.54 | Pubchem ID : | 735152 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P501-P261-P270-P271-P264-P280-P337+P313-P305+P351+P338-P362+P364-P332+P313-P301+P312+P330-P302+P352+P312-P304+P340+P312 | UN#: | N/A |
Hazard Statements: | H302+H312+H332-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 |
---|---|---|
95% | The mixture of diethyl malonate (80 ml, 0.5 mol) and sodium (2.76 g, 0.12 mol) was heated to 90 C in an oil bath and stirred for 1 h.After heating to 120 C for 45 min, it was cooled to room temperature.2-Chloro-4-nitropyridine (15.6 g, 0.1 mol) in toluene solution was added dropwise, and the reaction mixture was heated to 110 C for 1.5 h, cooled to room temperature and stirred for 15 h.The solvent was evaporated under reduced pressure, and then 6N hydrochloric acid (100 ml) was evaporated.The pH was made alkaline with a saturated sodium carbonate solution, extracted with ethyl acetate, combined with a base phase and dried over anhydrous sodium sulfate.Concentration by suction filtration gave 2-methyl-4-nitropyridine in a molar yield of 95%. | |
95% | The oil bath of the mixture of diethyl malonate (80 ml, 0.5 mol) and sodium (2.76 g, 0.12 mol) was warmed to 90 C. and stirred for 1 h. After warming to 120 C. and stirred for 45 min, it was cooled to room temperature.Add a solution of 2-chloro-4-nitropyridine (15.6g, 0.1mol) in toluene dropwise.The reaction solution was heated to 110 C for 1.5 h, cooled to room temperature and stirred for 15 h.The solvent was distilled off under reduced pressure, 6N hydrochloric acid (100ml) was added, the temperature was raised to reflux for 3.5h, and then cooled to room temperature.Adjust the pH to basic with saturated sodium carbonate solution, extract with ethyl acetate, combine the base phase,Dry over anhydrous sodium sulfate and concentrate by suction filtration to obtain 2-methyl-4-nitropyridine in a molar yield of 95%. |
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