Water → HCID 16751620, compound

3.0 g of 5-bromopyridin-2-ylamine in 5.8 ml of ethyl 2-bromoacetate are placed in a round-bottomed flask and stirred at ambient temperature for 48 h. A precipitate forms, and is recovered by filtration, washed with diethyl ether and oven-dried under reduced pressure. The solid is then taken up in 50 ml of ethanol, and 2.18 g of sodium hydrogencarbonate are added thereto. The reaction mixture is heated at the reflux of the solvent for 5 h, cooled to ambient temperature, and then concentrated under reduced pressure. The residue obtained is taken up between water and dichloromethane and the organic phase is separated, dried and concentrated under reduced pressure. 1.46 g of compound, used as it is in the subsequent stages, are obtained.

1. filtrationA precipitate forms, and is recovered by filtration
2. washwashed with diethyl ether
3. customoven-dried under reduced pressure
4. addition2.18 g of sodium hydrogencarbonate are added
5. temperatureThe reaction mixture is heated at the
6. temperaturereflux of the solvent for 5 h
7. temperaturecooled to ambient temperature
8. concentrationconcentrated under reduced pressure
9. customThe residue obtained
10. customthe organic phase is separated
11. customdried
12. concentrationconcentrated under reduced pressure
13. customare obtained

ORD record

ord-919d716d30154bc8b8a0bfaece5eabf3

Source dataset

uspto-grants-2012_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08338451B2