Hydrochloric Acid → 5,6,7,8-Tetrahydro-[1,2,4]triazolo[1,5-A]pyridin-2-amine

HRID 638850노트

반응식

HRID 638850 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]=12

참가 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

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated under reduced pressure
  3. additionThe residue was treated with saturated potassium carbonate solution
  4. extractionextracted with chloroform
  5. dry with materialThe organic layer was dried (Na2SO4)
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d19c284a06c14546b6128bf1ff07a41c
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691842B2

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