Synthetic Route of 59782-90-0, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 59782-90-0 as follows.
Under the protection of nitrogen, into the three-necked flask, add 53g benzylamine. Then use ice-bath to cool to 3 C. Then continue to add dropwise n-propanal 28g. Control dropwise addition time to 1h. Then add dropwise in batches 13g mass concentration of 10% KOH. Add dropwise 3 time. Then allow the layers to separate. To the organic phase, add 5g mass concentration of 10% KOH. Allow to stand overnight to prepare N-propylidenebenzylamine; Into a 250 ml four-necked flask, add 68g of the above-mentioned prepared N-propylidenebenzylamine. Then add 105 ml dichloromethane and triethylamine 47g. Stir and cool to 0 C, Then continue adding dropwise chloroacetyl chloride 57g. Control the dropwise addition at 1h. Then elevate temperature to 20 C. Continue reacting for 10 min; After the reaction is finished, the deionized water washing and the mass fraction of 10% hydrochloric acid pickling and the mass concentration is 10% of sodium hydroxide caustic wash, finally by reduced pressure distillation to remove the solvent, the reaction liquid prepared, subsequently heating the reaction liquid to column chromatography separation, collection acyl compound; In a 250 ml three-necked flask, add 23g dimethylformamide and 100 ml of 1,2-dichloromethane. Then stir and cool to 0 C. Then take 5.8g triphosgene. Use 50 ml of 1,2-dichloroethane to dissolve. Then add dropwise to the three-necked flask. Control the dropwise addition at 1h. After the completion of the dropwise addition, continue adding dropwise 4.4g of above-mentioned prepared acyl compound. Heat to 55 C and stir reaction for 1h; After the completion of reaction, washing with a large amount of deionized water and collecting the organic phase, for mass fraction of 10% sodium hydroxide solution to adjust the pH to 8.0, subsequently to its hierarchical collection of the organic layer, the solvent is removed by reduced pressure distillation column chromatography separation thereof, to collect colorless transparent crystal 2,3-dichloro-5-methylpyridine; 123.1g of nicotinic acid and 10 ml of 2,3-dichloro-5-methylpyridine were stirred and mixed; Elevate temperature to 55 C. Then add 270g phosphorus trichloride. At 70 C, enter chlorine gas for 2h. Continue heating to 150 C. Then 600 ml ethyl acetate and 20g sodium carbonate were added to the above-mentioned solution. Then continue reaction for 2h. Dry and concentrate and then dissolve in 100 ml toluene. Heat to 80 C and slowly enter phosgene. After reacting for 2h, the sodium carbonate is used to adjust the pH to 7.0, and separating an organic layer to dry the same, subsequently prepared desolution of the 2,3-chloro-5-chloromethyl pyridine.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,59782-90-0, its application will become more common.
Reference:
Patent; Changzhou University; Chen, Xingquan; (6 pag.)(2016);,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem