Stannous Chloride → 2,5-Dibromopyridin-3-amine

Temperatur

80 °C

To the solution of 2,5-Dibromo-3-nitro-pyridine (10.30 g, 35.47 mmol) in the 100 ml of ethanol was added SnCl2 (24.0 g, 106.42 mmol) slowly. The reaction mixture was heated at 80° C. for 2 h. After the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure. Water (250 mL) was added, white solid separated out, then, basified the reaction mixture with NaOH Solution. To this added the 250 ml of ethyl acetate. Filtered it and washed the residue with ethyl acetate, layers are separated, dried (Na2SO4), filtered, concentrated to give the desired product (6.20 g, 67.39%).

1. customAfter the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure
2. additionWater (250 mL) was added
3. customwhite solid separated out
4. additionTo this added the 250 ml of ethyl acetate
5. filtrationFiltered it
6. washwashed the residue with ethyl acetate, layers
7. customare separated
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated

ORD-Eintrag

ord-c271af90fdd74c5d8dee0187082e140a

Quelldatensatz

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08865736B2