Benzylamine → HCID 20222625, compound

Temperature

80 °C

59 g of benzylamine was added drop-by-drop over two hours to a stirred, refluxing mixture of 103 g of 1A, 50 ml of water and 200 ml of 100°/120° C. petroleum ether, under nitrogen, at 80° C., the pH of the mixture being maintained at 7-7.5. A solution of 40 g of sodium hydroxide in 60 ml of water was then added slowly to the stirred, refluxing mixture, at a rate sufficient to maintain the pH of the mixture at about 8. The resulting mixture was cooled and the aqueous phase was removed. The organic phase was washed with water, the solvent was evaporated under reduced pressure, and the residue was distilled in a wiped-film evaporator to give 1, as a colorless oil, b.p.: 80° C., 0.01 Torr.

1. temperaturerefluxing
2. temperaturerefluxing mixture
3. temperatureat a rate sufficient to maintain the pH of the mixture at about 8
4. temperatureThe resulting mixture was cooled
5. customthe aqueous phase was removed
6. washThe organic phase was washed with water
7. customthe solvent was evaporated under reduced pressure
8. distillationthe residue was distilled in a wiped-film evaporator
9. customto give 1

ORD record

ord-0ce2169cfe2941eaaeda28fd110d2417

Source dataset

uspto-grants-1987_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04634554