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Piperazine → 1-[4-(Trifluoromethyl)pyridin-2-yl]piperazine

HRID 270546
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인쇄 미리보기

반응식

HRID 270546 반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][N:3]=1.[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C(N(CC)CC)C>CN(C=O)C>[F:9][C:8]([F:11])([F:10])[C:6]1[CH:5]=[CH:4][N:3]=[C:2]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 4837PiperazineHCID 8471TriethylamineHCID 1449582-Chloro-4-(trifluoromethyl)pyridine

생성물 1

HCID 112184921-[4-(Trifluoromethyl)pyridin-2-yl]piperazine수율 43%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 2-chloro-4-(trifluoromethyl)pyridine (2.0 g, 11 mmol), piperazine (3 g, 30 mmol) and triethylamine (3.1 mL, 22 mmol) in DMF (10 mL) was heated at 100° C. overnight and concentrated in vacuo. The residue was purified by column chromatography on silica gel (EtOAc to EtOAc/MeOH/Et3N=9/1/0.5) to give 1.09 g (43%) of pure product. MS calculated for C10H12F3N3: (M+H) 232; found 232.1.

후처리

  1. concentrationconcentrated in vacuo
  2. customThe residue was purified by column chromatography on silica gel (EtOAc to EtOAc/MeOH/Et3N=9/1/0.5)

출처 및 근거

ORD 기록
ord-8569c7eace6c4438b8f31b8a191ede0c
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07449467B2

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