反应详情

An aqueous sodium nitrite solution (3.49 g of sodium nitrite in 12.5 mL of water) was dropwise added to a solution of 6-chloropyridine-3-amine (5.00 g) in hydrochloric acid (77.8 mL) over 10 minutes (such that the temperature does not exceed −20° C.) under dry ice-acetone cooling (−20 to −40° C.), followed by stirring under the same conditions for 1 hour. A solution of tin chloride (14.8 g) in hydrochloric acid (25 mL) was dropwise added thereto over 15 minutes, followed by stirring at approximately 0° C. for 2 hours. The precipitated solid was collected by filtration (washed with water and n-hexane) and was vacuum dried at 40° C. to yield the title compound (9.45 g, brown solid).

1. customdoes not exceed −20° C.
2. customunder dry ice-acetone cooling (−20 to −40° C.)
3. waitover 15 minutes
4. stirringby stirring at approximately 0° C. for 2 hours
5. filtrationThe precipitated solid was collected by filtration (washed with water and n-hexane)
6. customdried at 40° C.