Hydrochloric Acid → 2-(Piperazin-1-yl)pyridin-3-amine

HRID 1109917

반응식

HRID 1109917 반응식
[N:1]1([C:7]2[C:12]([N+:13]([O-])=O)=[CH:11][CH:10]=[CH:9][N:8]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl>C(O)C>[NH2:13][C:12]1[C:7]([N:1]2[CH2:2][CH2:3][NH:4][CH2:5][CH2:6]2)=[N:8][CH:9]=[CH:10][CH:11]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 37788341-(3-Nitropyridin-2-yl)piperazine

생성물 1

HCID 103973582-(Piperazin-1-yl)pyridin-3-amine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-(1-piperazinyl)-3-nitropyridine (24.50 g), ethanol (445 ml) and hydrochloric acid (1.2N, 44 ml) are combined and hydrogenated overnight at 40 psi, refilling when necessary. The mixture is filtered through celite, washed with ethanol, chloroform, ethanol and water. The organic solvents are removed with heat and reduced pressure. The remaining material is partitioned between methylene chloride (3×250 ml) and sodium bicarbonate. The organic layers are combined, dried over potassium carbonate, filtered and concentrated under reduced pressure to give an oil which slowly solidified upon standing to give 3-amino-2-(1-piperazinyl)pyridine.

후처리

  1. filtrationThe mixture is filtered through celite
  2. washwashed with ethanol, chloroform, ethanol and water
  3. customThe organic solvents are removed
  4. temperaturewith heat
  5. customThe remaining material is partitioned between methylene chloride (3×250 ml) and sodium bicarbonate
  6. dry with materialdried over potassium carbonate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customto give an oil which

출처 및 근거

ORD 기록
ord-343d5252f7814496892cffc6722115c9
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05322943

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