Piperazine → 1-(3-Fluoro-2-pyridinyl)piperazine

HRID 898722

反応式

HRID 898722 の反応式
Cl[C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[NH:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1>C(O)CCC>[F:8][C:7]1[C:2]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[N:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 4837PiperazineHCID 27827912-Chloro-3-fluoropyridine

生成物 1

HCID 1349871-(3-Fluoro-2-pyridinyl)piperazine収率 73%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
23 °C

実験手順

The product of Example 28A (3.3 g, 0.025 mol) in n-butanol (150 mL) at 23° C. was treated with piperazine (21.5 g, 0.25 mol) and then reflux for 3 days. The reaction mixture was allowed to cool to 23° C. and concentrated under reduced pressure. The residue was slurried with water and ethyl acetate. The ethyl acetate solution was separarted, dried over Na2SO4, filtered, and the filtrate concentrated under reduced pressure to afford 3.3 g (73% yield) of the title compound. 1H NMR (500 MHz, DMSO-d6) δ 2.80 (m, 4H), 3.38 (m, 4H), 6.84 (m, 1H), 7.47 (m, 1H), 7.98 (m, 1H); MS (ESI) m/e 182 (M+H)+.

後処理

  1. temperaturereflux for 3 days
  2. concentrationconcentrated under reduced pressure
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated under reduced pressure

出典と根拠

ORDレコード
ord-2ceda9972d994b22a1657fce47af09a7
出典データセット
uspto-grants-2008_04
特許番号
US07351828B2

関連ノート

読み込み中…