Urea → 2,2-Dimethylsuccinimide

HRID 423166노트

반응식

HRID 423166 반응식
[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]

참가 물질

4

반응물 2

HCID 1176UreaHCID 117012,2-Dimethylsuccinic acid

생성물 1

HCID 2256782,2-Dimethylsuccinimide수율 89.7%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
160 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-afc57db5b74d4b78be92e6daa89e28b4
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101753B2

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