Piperazine → 2-Methyl-4-piperazin-1-yl-7-(trifluoromethyl)quinoline

HRID 333958

반응식

HRID 333958 반응식
[CH3:1][C:2]1[CH:11]=[C:10](Cl)[C:9]2[C:4](=[CH:5][C:6]([C:13]([F:16])([F:15])[F:14])=[CH:7][CH:8]=2)[N:3]=1.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>COCCCOCCCO>[CH3:1][C:2]1[CH:11]=[C:10]([N:17]2[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]2)[C:9]2[C:4](=[CH:5][C:6]([C:13]([F:16])([F:15])[F:14])=[CH:7][CH:8]=2)[N:3]=1

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 47368054-Chloro-2-methyl-7-(trifluoromethyl)quinoline

생성물 1

HCID 668357982-Methyl-4-piperazin-1-yl-7-(trifluoromethyl)quinoline

시약·촉매·용매 1

HCID 669843-(3-Methoxypropoxy)-1-propanol용매

반응 조건

온도
140 °C

실험 절차

2-Methyl-4-chloro-7-(trifluoromethyl)quinoline (1.1 g, 4.4 mmol) was dissolved in dipropyleneglycolmonomethylether, piperazine was added (12 g, 14 mmol) and the mixture was stirred at 140° C. overnight. The solvent was removed under reduced pressure and the residue purified by column chromatography (prepacked silica column, gradient ethyl acetate/methanol with the addition of 1% ammonia) to yield 1.07 g of a solid. (3.6 mmol, 82%) MS (APCI): m/z=295.8 [M+1]+.

후처리

  1. customThe solvent was removed under reduced pressure
  2. customthe residue purified by column chromatography (prepacked silica column, gradient ethyl acetate/methanol
  3. additionwith the addition of 1% ammonia)

출처 및 근거

ORD 기록
ord-374e4806ed4545ceb827d566c07fdfb5
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883791B2

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