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

HRID 1061576

반응식

HRID 1061576 반응식
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

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 27827912-Chloro-3-fluoropyridine

생성물 1

HCID 1349871-(3-Fluoro-2-pyridinyl)piperazine수율 73%

시약·촉매·용매 1

HCID 2631-Butanol용매

반응 조건

온도
23 °C

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-4019cb29ea4941eabe33a20579df0c32
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06960589B2

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