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Undec-4-ene → Diethyl 2-oxopyrrolidine-5,5-dicarboxylate

HRID 260503
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HRID 260503 반응식
CCCCCCC=CCCC.Br[CH2:13][CH2:14][C:15]([NH:17][CH:18]([C:24]([O:26][CH2:27][CH3:28])=[O:25])[C:19]([O:21][CH2:22][CH3:23])=[O:20])=[O:16]>C(Cl)Cl>[O:16]=[C:15]1[CH2:14][CH2:13][C:18]([C:24]([O:26][CH2:27][CH3:28])=[O:25])([C:19]([O:21][CH2:22][CH3:23])=[O:20])[NH:17]1
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참가 물질

4

반응물 2

HCID 136496Undec-4-eneHCID 19045185Diethyl 2-(3-bromopropionamido)malonate

생성물 1

HCID 19045188Diethyl 2-oxopyrrolidine-5,5-dicarboxylate수율 37.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2(b) 314 μl of 1,8-diaza[5.4.0]-7-undecene were added to a solution of 620 mg of diethyl 2-(3-bromopropionamido)malonate (prepared as described above) dissolved in methylene chloride, and the mixture was stirred at room temperature for 3 hours. At the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure, poured into water and then extracted with diethyl ether. The extract was washed with 5% w/v aqueous hydrochloric acid, with a 5% w/v aqueous solution of sodium bicarbonate and with water, in that order, and dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure, to give a crude product. This was purified by column chromatography through silica gel, eluted with a 2:1 by volume mixture of cyclohexane and ethyl acetate, to give 171 mg of diethyl 2-oxopyrrolidine-5,5-dicarboxylate.

후처리

  1. concentrationAt the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure
  2. additionpoured into water
  3. extractionextracted with diethyl ether
  4. washThe extract was washed with 5% w/v aqueous hydrochloric acid, with a 5% w/v aqueous solution of sodium bicarbonate and with water, in that order
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was then removed by distillation under reduced pressure
  7. customto give a crude product
  8. customThis was purified by column chromatography through silica gel
  9. washeluted with a 2:1 by volume mixture of cyclohexane and ethyl acetate

출처 및 근거

ORD 기록
ord-5e6e85e2d9d8426d99779a089a22f9f3
출처 데이터셋
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05527905

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