Water → N~1~,N~1'~-(Ethane-1,2-diyl)di(ethane-1,2-diamine)--water (1/1)

Temperature

25 °C

520 g of commercial triethylenetetramine (starting purity 62%, GC in % area) are dissolved in 800 mL of toluene. 80 mL of water are added under stirring, the mixture is cooled at 25° C. and seeded with purified triethylenetetramine. The suspension is stirred for 45 min. at 20° C., then cooled at 5-10° C. for 1 h. The crystallized solid is filtered, washed with some toluene, then dried at 30° C. under vacuum for 8 h. 365 g of desired product are obtained. Yield: 91% on theoretical Water content: 17% GC: 97% (in % area)

1. stirringThe suspension is stirred for 45 min. at 20° C.
2. temperaturecooled at 5-10° C. for 1 h
3. filtrationThe crystallized solid is filtered
4. washwashed with some toluene
5. customdried at 30° C. under vacuum for 8 h

ORD record

ord-97e99f1de3144525a05e6522f872ee79

Source dataset

uspto-grants-2002_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06342597B1