Piperazine → 1-[6-(Trifluoromethyl)pyridin-2-yl]piperazine
반응식
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]([F:11])([F:10])[F:9])[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:4]1[N:3]=[C:2]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[CH:7]=[CH:6][CH:5]=1참가 물질
5
반응 조건
- 온도
- 100 °C
실험 절차
A solution of 2-chloro-6-(trifluoromethyl)pyridine (1.0 g, 5.5 mmol), piperazine (1.4 g, 16.0 mmol), and triethylamine (1.5 mL, 11.0 mmol) were mixed in DMF (10 mL) in a sealed tube. The mixture was heated at 100° C. overnight. The reaction mixture was concentrated and chromatographed on silica gel (ethyl acetate to EA/MeOH/Et3N=9:1:0.5) to give 1.05 g of the desired product. MS calculated for C10H12F3N3: (M+H) 232.1; found 232.1.
후처리
- concentrationThe reaction mixture was concentrated
- customchromatographed on silica gel (ethyl acetate to EA/MeOH/Et3N=9:1:0.5)
출처 및 근거
- ORD 기록
- ord-94679929560c47da93f23f3a88deb950
- 출처 데이터셋
- uspto-grants-2013_10
- 특허 번호
- US08563582B2
반응 노트
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