Ammonia → N-(2-Aminoethyl)ethyleneurea
Reaction equation
N[C:2](N)=[O:3].[NH2:5][CH2:6][CH2:7][NH:8][CH2:9][CH2:10][NH2:11].N>>[NH2:5][CH2:6][CH2:7][N:8]1[CH2:9][CH2:10][NH:11][C:2]1=[O:3]Participants
4
Conditions
- Temperature
- 140 °C
Procedure
In a suitable reactor equipped with agitation and a reflux condenser, 465 parts by weight of urea and 798 parts by weight of diethylenetriamine were charged. The reaction mix was slowly heated to 140° C. Ammonia started to evolve at about 130° C. The temperature was slowly raised to 150° C. As the evolution of ammonia subsided, vacuum was applied and the remaining ammonia was removed. Product yield was approximately 1000 parts by weight. The product had a viscosity of 6000 cps at 25° C. and an MEQ/g of 6.5. (MEQ=milliequivalent weight). Gel phase analysis of the product showed approximately 95% purity. The product can be used as is or further purified by vacuum distillation. The major impurity is unreacted diethylenetriamine.
Workup
- additionwere charged
- additionThe reaction mix
- customto evolve at about 130° C
- temperatureThe temperature was slowly raised to 150° C
- customthe remaining ammonia was removed
- customProduct yield
- customat 25° C.
- distillationfurther purified by vacuum distillation
Sources & evidence
- ORD record
- ord-e818cb7f3e9446be87f4df68f2020468
- Source dataset
- uspto-grants-1998_05
- Patent number
- US05746946
Reaction notes
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