Stannous Chloride → HCID 57429283, compound

Temperature

0 °C

To a suspension of 2-bromo-4-fluoroaniline in concentrated HCl (1.5M) at −10° C. was slowly added a 10.0M aqueous solution of NaNO2 (1.1 eq). The mixture was stirred at 0° C. for 2.5 hrs. A cold (−30° C.) solution of SnCl2 (3.8M) in concentrated HCl was then slowly added while maintaining the internal temperature below 10° C. The resulting mixture was stirred mechanically for 20 min at 0, then at room temperature for 1 hr. The thick slurry was filtered and the solid was air dried overnight. The solid was resuspended in cold HCl and filtered again. The dried material was suspended in Et2O, stirred for 10 min, filtered and air dried overnight to give the title compound as a beige solid.

1. temperaturewhile maintaining the internal temperature below 10° C
2. stirringThe resulting mixture was stirred mechanically for 20 min at 0
3. waitat room temperature for 1 hr
4. filtrationThe thick slurry was filtered
5. customdried overnight
6. filtrationfiltered again
7. stirringstirred for 10 min
8. filtrationfiltered
9. customair dried overnight

ORD record

ord-6b32a0e711f74e5bb71eed7d70731a86

Source dataset

uspto-grants-2006_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07019022B2