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ChemicalBook CAS DataBase List 1-(2-Aminoethyl)imidazolidin-2-one
6281-42-1

1-(2-Aminoethyl)imidazolidin-2-one synthesis

10synthesis methods
-

Yield: 96%

Reaction Conditions:

with ammonia at 125 - 160;Inert atmosphere;Large scale;Concentration;Temperature;

Steps:

1 Preparation of UDETA from DETA and Urea (R=1.5)
693 kg (6728 M) of DETA were introduced into a 1 m3 stirred reactor which has a double jacket, a device for introducing liquid, a nitrogen inerting system, a container and a scrubbing column for recovering the ammonia gas and the aqueous ammoniacal liquors. The reaction medium was brought to 130° C. while at the same time performing nitrogen sparging so as to deoxygenate the DETA. When the temperature was reached, the introduction of an aqueous solution of urea at 40%, on the basis of 671.4 kg (4476 M), was begun. The DETA:urea molar ratio was therefore 1.5:1.[0045]The urea was introduced fractionwise over the course of 4 h.[0046]The release of ammonia, which appeared at soon as the running-in began, was scrubbed on the scrubbing column and the aqueous ammoniacal liquors were collected in the container. The reaction mixture was then kept at 130° C. for 1 h30 in order to finish off the removal of the water.[0047]The reaction medium was then gradually heated by bringing it: to 140° C. for 45 min, then to 150° C. for 45 min, then to 160° C. for 5 h. It was cooled to 125° C. at the end of the reaction, and then the excess DETA was removed under reduced pressure of from 10 to 1.5 mbar and with mild nitrogen sparging, for a maximum of 5 h. The product obtained after returning the equipment to atmospheric pressure, cooling to 60° C. and withdrawal from the reactor had a UDETA titer of 95-96% and contained 1-2.5% of TETU

References:

Arkema France;Baloche, Alain;Gamet, Jean-Paul;Gillet, Jean-Philippe US2013/23667, 2013, A1 Location in patent:Paragraph 0044; 0045; 0046; 0047

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