Piperidine → 4-Piperidin-1-ylbenzonitrile

HRID 1505167ノート

反応式

HRID 1505167 の反応式
Cl[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[NH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1>>[N:10]1([C:2]2[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=2)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1

参加物

3

反応物 2

HCID 8082PiperidineHCID 121634-Chlorobenzonitrile

生成物 1

HCID 7667714-Piperidin-1-ylbenzonitrile収率 89%

反応条件

温度
100 °C

実験手順

To commercially available 4-chlorobenzonitrile 17 (1 g, 7.26 mmol) 3 ml of piperidine were added and the reaction was heated at 100° C. for 72 hours in closed vessel. The reaction was evaporated and the residue was dissolved in AcOEt and washed with water and brine. The purification of the crude residue by chromatographic column using AcOEt 1/Petroleum ether 9 as eluant gave 1.2 g of a pale yellow oil. Yield=89% 1HNMR (DMSO, 200 MHz) δ 1.57 (6H, m), 3.34 (4H, m), 6.98 (2H, d, J=9 Hz), 7.53 (2H, d, J=9 Hz)

後処理

  1. customThe reaction was evaporated
  2. dissolutionthe residue was dissolved in AcOEt
  3. washwashed with water and brine
  4. customThe purification of the crude residue by chromatographic column

出典と根拠

ORDレコード
ord-1e0c9dab523544ef9e18f4b8b5dc5e5c
出典データセット
uspto-grants-2015_12
特許番号
US09216975B2

反応ノート

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