Piperidine → HCID 67187268、化合物

HRID 451616ノート

反応式

HRID 451616 の反応式
F[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[C:7](=[O:12])[CH2:6][CH2:5]2.[NH:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1>N1C=CC=CC=1>[F:11][C:10]1[CH:9]=[C:8]2[C:4]([CH2:5][CH2:6][C:7]2=[O:12])=[CH:3][C:2]=1[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1

参加物

4

反応物 2

HCID 8082PiperidineHCID 117689445,6-Difluoro-1-indanone

生成物 1

HCID 67187268HCID 67187268、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

5,6-difluoro-indan-1-one (2.49 g, 14.8 mmol) and piperidine (4.4 ml, 3.78 g, 44.4 mmol) were dissolved in pyridine (10 ml) and heated to reflux for 16 hours. The reaction was cooled, and the solvent removed under vacuum. The residue was taken in ethyl ether, washed with 1N aqueous sodium hydroxide and water, dried with magnesium sulfate, and the solvent removed under vacuum to give the desired product as 2.97 g of a black solid that was used without further purification. 1H NMR (300 MHz, CDCl3) 7.32 (d, 1H), 6.88 (d, 1H), 3.19 (m, 4H), 3.03 (m, 2H), 2.66 (m, 2H), 1.73 (m, 4H), 1.62 (m, 2H). MS (CSI) m/e 234 (M+H)+

後処理

  1. temperatureheated
  2. temperatureto reflux for 16 hours
  3. temperatureThe reaction was cooled
  4. customthe solvent removed under vacuum
  5. washwashed with 1N aqueous sodium hydroxide and water
  6. dry with materialdried with magnesium sulfate
  7. customthe solvent removed under vacuum

出典と根拠

ORDレコード
ord-b394b8a175d84154a5a9758629da0424
出典データセット
uspto-grants-2013_07
特許番号
US08487116B2

反応ノート

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