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Dimethylformamide dimethyl acetal → (Z)-tert-butyl 3-((dimethylamino)methylene)-4-oxopyrrolidine-1-carboxylate

HRID 241559
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HRID 241559 반응식
[O:1]=[C:2]1[CH2:6][CH2:5][N:4]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:3]1.[CH3:14][N:15]([CH:17](OC)OC)[CH3:16]>>[CH3:14][N:15](/[CH:17]=[C:6]1/[CH2:5][N:4]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:3][C:2]/1=[O:1])[CH3:16]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 471360Tert-butyl 3-oxopyrrolidine-1-carboxylate

생성물 1

HCID 56971730(Z)-tert-butyl 3-((dimethylamino)methylene)-4-oxopyrrolidine-1-carboxylate

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온도
105 °C

실험 절차

A solution of tert-butyl 3-oxopyrrolidine-1-carboxylate (40 g, 216 mmol) was treated with DMF-DMA (267 g, 2241 mmol) and heated at 105° C. for 40 min. The solution was cooled and evaporated under reduced pressure and the resulting orange solid was treated with hexane (200 mL) and cooled in the refrigerator over the weekend. The resulting brownish-yellow solid was collected by filtration, dried and used in the next setp without further purification.

후처리

  • temperatureThe solution was cooled
  • customevaporated under reduced pressure
  • additionthe resulting orange solid was treated with hexane (200 mL)
  • temperaturecooled in the refrigerator over the weekend
  • filtrationThe resulting brownish-yellow solid was collected by filtration
  • customdried
  • customused in the next setp without further purification
  • 출처 및 근거

    ORD 기록
    ord-d4c023be3a88447cba0dadf38f9eed83
    출처 데이터셋
    uspto-grants-2014_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08653059B2

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