Acetic Anhydride → 1-(4-(4-bromo-1H-pyrazol-1-yl)piperidin-1-yl)ethanone

HRID 2400331노트

반응식

HRID 2400331 반응식
Cl.[Br:2][C:3]1[CH:4]=[N:5][N:6]([CH:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH:7]=1.[C:14](OC(=O)C)(=[O:16])[CH3:15]>N1C=CC=CC=1>[Br:2][C:3]1[CH:4]=[N:5][N:6]([CH:8]2[CH2:13][CH2:12][N:11]([C:14](=[O:16])[CH3:15])[CH2:10][CH2:9]2)[CH:7]=1

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 534078484-(4-bromo-1H-pyrazol-1-yl)piperidine hydrochloride

생성물 1

HCID 593926411-(4-(4-bromo-1H-pyrazol-1-yl)piperidin-1-yl)ethanone수율 81.3%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
40 °C

실험 절차

To a solution of 4-(4-bromopyrazol-1-yl)piperidine hydrochloride (300 mg, 1.13 mmol) in pyridine (3 ml) was added acetic anhydride (0.107 ml, 1.13 mmol) under an inert atmosphere. The reaction was stirred at 40° C., until reaction complete then evaporated under reduced pressure and re-evaporated with toluene twice, then partitioned between water and EtOAc. The organic layer was washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure to give the product (250 mg), which was used without further purification MS: [M+H]+=272

후처리

  1. customevaporated under reduced pressure
  2. customre-evaporated with toluene twice
  3. custompartitioned between water and EtOAc
  4. washThe organic layer was washed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-4cc8b5081cb04140b2a1104b5bc99375
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08796244B2

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