Acetone → Ethylenebismaleimide

HRID 262419

反応式

HRID 262419 の反応式
[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]

参加物

8

反応物 5

HCID 180Acetone2 回HCID 3301EthylenediamineHCID 7918Acetic AnhydrideHCID 7923Maleic AnhydrideHCID 24644Magnesium chloride hexahydrate

生成物 1

HCID 237509Ethylenebismaleimide収率 27%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8471Triethylamine溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4e1c03fd2c6f454490ca464d71c987bf
出典データセット
uspto-grants-1979_05
特許番号
US04154737

関連ノート

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