Ethylenediamine → N1-octylethane-1,2-diamine

50 g (0.83 mol) of anhydrous ethylenediamine, 31.2 g (0.21 mol) of octyl chloride and 400 ml of ethanol were mixed and refluxed 6 hours under heating. After evaporation of ethanol under reduced pressure, the lower layer was removed and 200 ml of benzene and 100 ml of water were added to the upper layer for full rinsing. The benzene fraction was dried over anhydrous sodium sulfate, concentrated and then cooled to precipitate crystals. After filtering, crystals were redissolved into 200 ml of benzene and the solution was fully rinsed with water. After being dried over anhydrous sodium sulfate, the benzene solution was concentrated and cooled to precipitate crystals. After filtration, crystals were washed with a small volume of methanol.

1. temperaturerefluxed 6 hours
2. temperatureunder heating
3. customAfter evaporation of ethanol under reduced pressure
4. customthe lower layer was removed
5. addition200 ml of benzene and 100 ml of water were added to the upper layer for full rinsing
6. dry with materialThe benzene fraction was dried over anhydrous sodium sulfate
7. concentrationconcentrated
8. temperaturecooled
9. customto precipitate crystals
10. filtrationAfter filtering
11. dissolutioncrystals were redissolved into 200 ml of benzene
12. washthe solution was fully rinsed with water
13. dry with materialAfter being dried over anhydrous sodium sulfate
14. concentrationthe benzene solution was concentrated
15. temperaturecooled
16. customto precipitate crystals
17. filtrationAfter filtration, crystals
18. washwere washed with a small volume of methanol

ORD record

ord-301deee3b77c493db0c345a663343e87

Source dataset

uspto-grants-1983_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04421846