Acetone → 1H-Pyrrole-2,5-dione, 1,1'-(4-methyl-1,3-phenylene)bis-

HRID 262418

반응식

HRID 262418 반응식
[C:1]1(=[O:7])O[C:4](=[O:5])[CH:3]=[CH:2]1.[CH3:8][C:9]1[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][C:10]=1[NH2:16].O.O.O.O.O.O.[Cl-].[Mg+2].[Cl-].C(O[C:30](=[O:32])[CH3:31])(=O)C.[CH3:33][C:34](C)=[O:35]>O.C(N(CC)CC)C>[CH3:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]2[C:30](=[O:32])[CH:31]=[CH:33][C:34]2=[O:35])=[CH:11][C:10]=1[N:16]1[C:1](=[O:7])[CH:2]=[CH:3][C:4]1=[O:5]

참가 물질

8

반응물 5

HCID 180Acetone2회HCID 72612,4-DiaminotolueneHCID 7918Acetic AnhydrideHCID 7923Maleic AnhydrideHCID 24644Magnesium chloride hexahydrate

생성물 1

HCID 808931H-Pyrrole-2,5-dione, 1,1'-(4-methyl-1,3-phenylene)bis-수율 85%

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 (1.7 parts) in 3.9 parts acetone was added a solution of 1 part 4-methyl-m-phenylenediamine, 0.28 part triethylamine and 2.5 parts acetone. The heterogeneous reaction mixture was stirred at 40° C. for 30 minutes. Magnesium chloride hexahydrate (0.071 part) and 2.16 part acetic anhydride were added all at once. The reaction temperature was raised to 50° C. and maintained for 2.5 hours. Thirty minutes after the addition the mixture became homogeneous and remained so. The solution was cooled, and 16 parts water was added; the precipitated product was filtered by vacuum filtration, washed with water, and dried in a vacuum oven at 60° C. for 24 hours. N,N'-(4-Methyl-m-phenylene)dimaleimide, m.p. 168°-172° C., was obtained in 85% yield.

후처리

  1. customA flask was equipped as in Example 1
  2. temperatureThe reaction temperature was raised to 50° C.
  3. temperaturemaintained for 2.5 hours
  4. additionThirty minutes after the addition the mixture
  5. temperatureThe solution was cooled
  6. filtrationthe precipitated product was filtered by vacuum filtration
  7. washwashed with water
  8. customdried in a vacuum oven at 60° C. for 24 hours

출처 및 근거

ORD 기록
ord-42c1bcf76c544651a422c1274a989376
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04154737

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