Tetrabutylammonium Fluoride → 2-Ethenylpiperidin-4-one

HRID 1510158노트

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HRID 1510158 반응식
[O:1]=[C:2]1[CH2:7][CH2:6][N:5](C(OCC[Si](C)(C)C)=O)[CH:4]([CH:17]=[CH2:18])[CH2:3]1.CCCC[N+](CCCC)(CCCC)CCCC.[F-]>O1CCCC1>[CH:17]([CH:4]1[CH2:3][C:2](=[O:1])[CH2:7][CH2:6][NH:5]1)=[CH2:18]

참가 물질

4

반응물 2

HCID 2724141Tetrabutylammonium FluorideHCID 667904002-(Trimethylsilyl)ethyl 4-oxo-2-vinylpiperidine-1-carboxylate

생성물 1

HCID 205693092-Ethenylpiperidin-4-one

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

2-(trimethylsilyl)ethyl 4-oxo-2-vinylpiperidine-1-carboxylate (24.1 g, 89.0 mmol) was dissolved in tetrahydrofuran (90 ml) at 0° C. and added TBAF (268 ml, 268 mmol) dropwise. The solution stirred at 0° C. for 30 min then at rt for an additional three hrs. The solution was quenched with 1N HCl and extracted five times with EtOAc. The organic fractions were combined, dried with Na2SO4, and concentrated. The crude product was not purified.

후처리

  1. waitat rt for an additional three hrs
  2. customThe solution was quenched with 1N HCl
  3. extractionextracted five times with EtOAc
  4. dry with materialdried with Na2SO4
  5. concentrationconcentrated
  6. customThe crude product was not purified

출처 및 근거

ORD 기록
ord-fbf73bb80b2548a88a9662d0c6031966
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08211904B2

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