Urea → 2,2-Dimethylsuccinimide

HRID 14581ノート

反応式

HRID 14581 の反応式
[CH3:1][C:2]([CH3:10])([C:7](O)=[O:8])[CH2:3][C:4](O)=[O:5].[NH2:11]C(N)=O>O>[CH3:1][C:2]1([CH3:10])[CH2:3][C:4](=[O:5])[NH:11][C:7]1=[O:8]

参加物

4

反応物 2

HCID 1176UreaHCID 117012,2-Dimethylsuccinic acid

生成物 1

HCID 2256782,2-Dimethylsuccinimide収率 89.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
160 °C

実験手順

The mixture of 10 g of 3,3-dimethylsuccinic acid and 102.7 g of urea was stirred for 10 hours at 160° C. Into the reaction mixture was added water at 100° C., and the mixture was cooled to near room temperature. The mixture was extracted with ethyl acetate three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 7.8 g of 3,3-dimethylpyrrolidin-2,5-dione.

後処理

  1. temperaturethe mixture was cooled to near room temperature
  2. extractionThe mixture was extracted with ethyl acetate three times
  3. washThe organic layers were washed with a saturated sodium chloride aqueous solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-bfec5973ad2643fa973dabb9e9e42e5e
出典データセット
uspto-grants-2010_06
特許番号
US07732448B2

反応ノート

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