462-08-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 462-08-8, name is Pyridin-3-amine, molecular formula is C5H6N2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
50.0 g (0.53 mol) of 3-aminopyridine was added to 34.9 g of 35percent hydrochloric acid and stirred to prepare an aqueous hydrochloric acid solution of 3-aminopyridine. In addition, 35.9 g (0.52 mol, 0.98 mol equivalent to 3-aminopyridine) of sodium nitrite was added to 54.0 g of water and stirred to prepare an aqueous solution of sodium nitrite. 131 g of hydrochloric acid was placed in a 500 mL four-necked brown colben and cooled to -20 ¡ã C. An aqueous hydrochloric acid solution of 3-aminopyridine and an aqueous solution of sodium nitrite were simultaneously added dropwise to hydrochloric acid in a temperature range of -20 ¡À 2 ¡ã C. over 2 hours with stirring. After completion of the dropwise addition, the mixture was further stirred for 30 minutes in a temperature range of -20 ¡À 2 ¡ã C. to obtain an aqueous solution of pyridine-3-diazonium salt650 g of dichloromethane was placed in 1000 mL four-necked brown bottle and cooled to 0 ¡ã C., and 119 g (1.86 mol) of sulfur dioxide gas was blown into the solution to dissolve. 0.9 g (0.006 mol) of copper (II) chloride dihydrate was added and cooled to -5 ¡ã C., and an aqueous solution of pyridine-3-diazonium salt was added over a period of 1 hour at a temperature range of -5 ¡À 2 ¡ã C. Was added dropwise. After completion of the dropwise addition, the mixture was further stirred for 1 minute at a temperature range of -5 ¡À 2 ¡ã C. The copper catalyst was removed by filtration while maintaining the temperature of the reaction solution at -5 ¡À 5 ¡ã C., and then the organic layer and the aqueous layer were separated. It was extracted with 195 g of dichloromethane ¡Á 3 times at a temperature of -5 ¡À 5 ¡ã C. and mixed all together to obtain 1353 g of an organic layer. GC analysis of this organic layer revealed that the concentration of pyridine-3-sulfonyl chloride was 3.76percent by mass and the yield was 54.0percent. The obtained organic layer was washed with 50 g of water while maintaining the temperature at 3 ¡À 2 ¡ã C., and then dehydrated using 20 g of magnesium sulfate at room temperature. After removing the magnesium sulfate by filtration, the filtrate was concentrated under reduced pressure (30 to 35 ¡ã C.,> 67 kPa) to remove dichloromethane. Subsequently, distillation under reduced pressure (110 ¡ã C., 1.3 kPa) gave 49.0 g (0.276 mol, yield 52.1percent) of pyridine-3-sulfonyl chloride.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 462-08-8, Pyridin-3-amine, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; Tama Chemical Industry Co., Ltd.; Nobushima, Hirofumi; Kobayashi, Hitoshi; (9 pag.)JP2016/175885; (2016); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem