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ChemicalBook CAS DataBase List 3-Cyanopyridine

3-Cyanopyridine synthesis

11synthesis methods
-

Yield:100-54-9 99%

Reaction Conditions:

with ammonium sulphate;anhydrous sodium carbonate;sulphur in dimethyl sulfoxide at 120; for 10 h;Sealed tube;

Steps:

24 Example 24

Combine 3-pyridinecarboxaldehyde (54.0mg, 0.5mmol), ammonium sulfate (66.1mg, 0.5mmol), sodium carbonate (53.0mg, 0.5mmol),Sulfur powder (32.0 mg, 1 mmol) and 0.5 ml of solvent DMSO were put into the reaction tube, and the reaction tube was sealed. The reaction tube was placed in a 120°C oil bath reaction pot with magnetic stirring for 10 hours. After cooling to room temperature. Then it was extracted with ethyl acetate and the organic phases were combined. The organic phase was washed with saturated brine, and after liquid separation, the organic phase was dried with anhydrous sodium sulfate,After filtering and concentrating the filtrate under reduced pressure, the pure product was separated by thin layer chromatography using ethyl acetate: petroleum ether=1:10 (volume ratio) as the developing solvent. White solid, 99% yield.

References:

CN111606823,2020,A Location in patent:Paragraph 0076; 0077

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