참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethylenediamine | HCID 3301 | — |
| 반응물 | Methyl 7-oxabicyclo[2.2.1]hept-5-ene-2-carboxylate | HCID 12271748 | — |
| 생성물 | 2-Propenamide, N,N'-1,2-ethanediylbis- | HCID 168964 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04605740 |
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| 출처 데이터셋 | uspto-grants-1986_08 |
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| ORD ID | ord-2180f63ff21347468aa6fc113cb93506 |
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| 출처 메모 | uspto-grants-1986_08 |
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