Ethylenediamine → 2-Propenamide, N,N'-1,2-ethanediylbis-

温度

140 °C

7.2 parts 30% methanolic Na-methylate solution are added to 15 parts ethylenediamine. 77 parts 2-carbomethoxy-7-oxabicyclo(2,2,1)hept-5-ene are added drop-wise at 30° C. during cooling. Recrystallisation is then allowed to proceed overnight and the crystalline mass is dissolved in 400 parts chloroform, and neutralised with 4 parts concentrated hydrochloric acid. 50 parts water are added, the organic phase separated off, and the aqueous phase extracted 5 times with 50 parts chloroform in each instance. The combined organic phases are reduced in a rotary evaporator at a bath temperature of 90° C. and under a vacuum of 20 Torr. The residue is heated in a vacuum of 10 Torr to 110° to 120° C. (bath temperature 140° C.). On conclusion of the furane separation the sedimentation temperature increases to 140° C. After cooling, the product is dissolved in hot n-butanol, filtered, and allowed to recrystallise at 0° C. 27 g N,N'-ethylenebisacrylamide with a melting point of 150° to 155° C. is obtained.

1. temperatureduring cooling
2. customRecrystallisation
3. dissolutionthe crystalline mass is dissolved in 400 parts chloroform
4. addition50 parts water are added
5. customthe organic phase separated off
6. extractionthe aqueous phase extracted 5 times with 50 parts chloroform in each instance
7. customThe combined organic phases are reduced in a rotary evaporator at a bath temperature of 90° C.
8. customOn conclusion of the furane separation the sedimentation temperature
9. temperatureincreases to 140° C
10. temperatureAfter cooling
11. dissolutionthe product is dissolved in hot n-butanol
12. filtrationfiltered
13. customto recrystallise at 0° C

ORDレコード

ord-2180f63ff21347468aa6fc113cb93506

出典データセット

uspto-grants-1986_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04605740