Hydrochloric Acid → 5,6,7,8-Tetrahydro-[1,2,4]triazolo[1,5-A]pyridin-2-amine
반응식
Cl.[N:2]1[C:3]([NH2:11])=[N:4][N:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=12>C(O)C.[Pd]>[N:2]1[C:3]([NH2:11])=[N:4][N:5]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=12참가 물질
5
실험 절차
The 12.7% solution of HCl in ethanol (5.35 mL) and 10% Pd—C (50% wet) (2.5 g) were added to the mixture of [1,2,4]triazolo[1,5-a]pyridin-2-ylamine (2.5 g) in ethanol (72 mL). The reaction mixture was hydrogenated at 400 KPa of H2 for 3 days at room temperature. The mixture was filtered and concentrated under reduced pressure. The residue was treated with saturated potassium carbonate solution and extracted with chloroform. The organic layer was dried (Na2SO4) and concentrated under reduced pressure. The title compound was obtained as a pale yellow solid (2.31 g, 90%). 1H-NMR (400 MHz, CDCl3) δ 1.88-1.94 (m, 2H), 1.98-2.05 (m, 2H), 2.77 (t, 2H, J=6.2 Hz), 3.95 (t, 2H, J=6.2 Hz), 4.09 (brs, 2H).
후처리
- filtrationThe mixture was filtered
- concentrationconcentrated under reduced pressure
- additionThe residue was treated with saturated potassium carbonate solution
- extractionextracted with chloroform
- dry with materialThe organic layer was dried (Na2SO4)
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-d19c284a06c14546b6128bf1ff07a41c
- 출처 데이터셋
- uspto-grants-2010_04
- 특허 번호
- US07691842B2
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