Dichloromethane → 3-(Trifluoromethyl)-5,6,7,8-tetrahydro-(1,2,4)triazolo(4,3-a)pyrazine
반응식
[F:1][C:2]([F:13])([F:12])[C:3]1[N:7]2[CH:8]=[CH:9][N:10]=[CH:11][C:6]2=[N:5][N:4]=1.ClCCl>[Pd].C(O)C>[F:12][C:2]([F:1])([F:13])[C:3]1[N:7]2[CH2:8][CH2:9][NH:10][CH2:11][C:6]2=[N:5][N:4]=1참가 물질
5
실험 절차
3-(Trifluoromethyl)-1,2,4-triazolo[4,3-α]pyrazine (540 mg, 2.87 mmol, from Step A) was hydrogenated under atmospheric hydrogen with 10% Pd/C (200 mg) as a catalyst in ethanol (10 mL) at ambient temperature for 18 h. Filtration through Celite followed by concentration gave a dark colored oil. Dichloromethane was added to the above oil and the insoluble black precipitate was filtered off. Concentration of the filtrate gave the title compound as an oil (495 mg). 1H NMR (500 MHz, CDCl3) δ 2.21 (br, 1H), 3.29 (t, 2H, J=5.5 Hz), 4.09 (t, 2H, J=5.5 Hz), 4.24 (s, 2H). LC/MS (M+1) 193.
후처리
- filtrationFiltration through Celite
- concentrationfollowed by concentration
- customgave a dark colored oil
- filtrationthe insoluble black precipitate was filtered off
출처 및 근거
- ORD 기록
- ord-ceed90d4c91c4d838d852b3b6cb80165
- 출처 데이터셋
- uspto-grants-2006_10
- 특허 번호
- US07125873B2
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