Ethyl Acetate → 5,6,7,8-Tetrahydro-2-(trifluoromethyl)[1,2,4]triazolo[1,5-a]pyrazine
반응식
[F:1][C:2]([F:13])([F:12])[C:3]1[N:11]=[C:6]2[CH:7]=[N:8][CH:9]=[CH:10][N:5]2[N:4]=1.C(OCC)(=O)C.CO.ClCCl>[Pd].C(O)C>[F:12][C:2]([F:1])([F:13])[C:3]1[N:11]=[C:6]2[CH2:7][NH:8][CH2:9][CH2:10][N:5]2[N:4]=1참가 물질
6
실험 절차
2-(Trifluoromethyl)-[1,2,4]triazolo[1,5-a]pyrazine (340 mg, 1.81 mmol, from Step C) was hydrogenated under atmospheric hydrogen with 10% palladium on carbon (60 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. Flash chromatography (100% ethyl acetate, then 10% methanol/dichloromethane) gave the title compound as a white solid. 1H-NMR (500 MHz, CDCl3): δ 1.80 (br, 1H), 3.40 (t, 2H, J=5.5 Hz), 4.22-4.26 (m, 4H); LC/MS 193 (M+1).
후처리
- filtrationFiltration through Celite
- concentrationfollowed by concentration
- customgave a dark colored oil
출처 및 근거
- ORD 기록
- ord-10c812d188e84d03956c5b2778ed4268
- 출처 데이터셋
- uspto-grants-2009_01
- 특허 번호
- US07482336B2
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