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

HRID 2400331ノート

反応式

HRID 2400331 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
40 °C

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-4cc8b5081cb04140b2a1104b5bc99375
出典データセット
uspto-grants-2014_08
特許番号
US08796244B2

反応ノート

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