preparation of 3-pyridinecarboxaldehyde_industrial additives

preparation background and overview of 3-pyridinecarboxaldehyde

as an important pharmaceutical intermediate and fine chemical raw material, 3-pyridinecarboxaldehyde has a wide range of applications and broad market prospects. in medicine, 3-pyridinecarboxaldehyde, as an important pharmaceutical intermediate, can be used to synthesize the laxative bisacodyl and is also a raw material for the synthesis of the organophosphate antidote pralidoxime. recently, it has been reported that 3-pyridinecarboxaldehyde can also be used to synthesize the laxative bisacodyl. raw material for anti-hiv protease inhibitors; in agriculture, 3-pyridinecarboxaldehyde is a necessary intermediate for the synthesis of aminoguanidine bicarbonate of some acaricides; in the photosensitive industry, 3-pyridinecarboxaldehyde can be used to synthesize nitrogen-containing heterocyclic colors photographic materials.

preparation of 3-pyridinecarboxaldehyde

3-methylpyridine reacts with glacial acetic acid and hydrogen peroxide. the reaction temperature is 63°c and the reaction time is 17h. the molar ratio of 3-methylpyridine, glacial acetic acid and hydrogen peroxide is 1:4:3.5, and 3-methylpyridine is obtained. pyridine nitrogen oxide; 3-pyridine nitrogen oxide reacts with acetic anhydride, the reaction temperature is 92°c, the reaction time is 4h, the molar ratio of the 3-pyridine nitrogen oxide and acetic anhydride is 1:2.3, and acetic acid-3 is obtained -pyridine methyl ester; 3-pyridine methyl acetate reacts with potassium hydroxide solution. the reaction time is 5 hours. the molar ratio of 3-pyridine methyl acetate to potassium hydroxide is 1:1.8. the reaction gives 3-pyridine. methanol; 3-pyridinemethanol is cooled with ice water and pcc is added. the molar ratio of 3-pyridinemethanol to pcc is 1:2.5, and the temperature is 2°c; then the reaction is carried out at room temperature, the temperature is 23°c, and monitored by thin layer chromatography. complete reaction.

preparation and application of 3-pyridinecarboxaldehyde

cn201811091233.1 discloses a preparation method of cordil nipyridinyl acetate, which includes the following steps: synthesis of 3-pyridine oxazolidine: add aminoethanol to the alcohol solution of 3-pyridine carbaldehyde under stirring and solid brominated reagent, stir at room temperature until 3-pyridinecarboxaldehyde is consumed; quench the reaction system with a saturated solution of sodium thiosulfate, extract with ethyl acetate, and concentrate the organic phase to obtain crude 3-pyridineoxazolidine; nicol synthesis of dil: dissolve 3-pyridine oxazolidine in a solvent, then add nitrite, heat, add oxygen-containing gas, stir until 3-pyridine oxazolidine is consumed; quench with saturated sodium sulfate solution , extracted with ethyl acetate, concentrated, and the crude product was dissolved with 30% ethyl acetate in n-hexane solution, cooled to 10 degrees, solid precipitated, filtered, and nicorandil was obtained.

references

[1] [chinese invention] cn201911167747.5 a synthesis method of 3-pyridinecarboxaldehyde

[2] cn201811091233.1 preparation method of nicorandil