Urea → 2,2-Dimethylsuccinimide

HRID 423166ノート

反応式

HRID 423166 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

10 g of 3,3-dimethyl succinic acid and 102.7 g of urea were mixed and stirred at 160° C. for 10 hours. Then water was added to the reaction mixture which was cooled to about 100° C., and further cooled to about room temperature, then extracted with ethyl acetated three times. The organic layers were joined, washed with saturated aqueous solution of sodium chloride, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 7.8 g of 3,3-dimethyl-2,5-pyrrolidine dion.

後処理

  1. temperaturewas cooled to about 100° C.
  2. temperaturefurther cooled to about room temperature
  3. extractionextracted with ethyl
  4. washwashed with saturated aqueous solution of sodium chloride
  5. dry with materialdried with anhydrous magnesium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-afc57db5b74d4b78be92e6daa89e28b4
出典データセット
uspto-grants-2012_01
特許番号
US08101753B2

反応ノート

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