Acetone → Ethylenebismaleimide

HRID 262419

반응식

HRID 262419 반응식
[C:1]1(=[O:7])O[C:4](=[O:5])[CH:3]=[CH:2]1.[CH2:8]([NH2:11])[CH2:9][NH2:10].O.O.O.O.O.O.[Cl-].[Mg+2].[Cl-].C(O[C:25](=[O:27])[CH3:26])(=O)C.[CH3:28][C:29](C)=[O:30]>O.C(N(CC)CC)C>[CH2:8]([N:11]1[C:1](=[O:7])[CH:2]=[CH:3][C:4]1=[O:5])[CH2:9][N:10]1[C:25](=[O:27])[CH:26]=[CH:28][C:29]1=[O:30]

참가 물질

8

반응물 5

HCID 180Acetone2회HCID 3301EthylenediamineHCID 7918Acetic AnhydrideHCID 7923Maleic AnhydrideHCID 24644Magnesium chloride hexahydrate

생성물 1

HCID 237509Ethylenebismaleimide수율 27%

시약·촉매·용매 2

HCID 962Water용매HCID 8471Triethylamine용매

반응 조건

온도
40 °C

실험 절차

A flask was equipped as in Example 1. To a solution of maleic anhydride (3.64 parts) in 10.6 parts acetone was added a solution of 1 part ethylenediamine, 0.61 part triethylamine and 1.5 parts acetone over a 25-minute period. The resulting reaction mixture contained white solids and was maintained at 40° C. for 30 minutes. Magnesium chloride hexahydrate (0.15 part) and 4.6 parts acetic anhydride were added all at once. The reaction temperature was raised to 50° C. and held there for 2.5 hours. The homogeneous reaction mixture was cooled and 25 parts water added. The precipitated product was filtered by vacuum filtration, washed with water, and dried in a vacuum oven. A 27% yield of N,N'-ethylenedimaleimide, m.p. 193°-194° C., was obtained.

후처리

  1. customA flask was equipped as in Example 1
  2. customThe resulting reaction mixture
  3. temperatureThe reaction temperature was raised to 50° C.
  4. temperatureThe homogeneous reaction mixture was cooled
  5. filtrationThe precipitated product was filtered by vacuum filtration
  6. washwashed with water
  7. customdried in a vacuum oven

출처 및 근거

ORD 기록
ord-4e1c03fd2c6f454490ca464d71c987bf
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04154737

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