1-(6-Nitro-pyridin-3-yl)-azetidin-3-ol → 1-(6-Aminopyridin-3-yl)azetidin-3-ol

HRID 407770노트

반응식

HRID 407770 반응식
[N+:1]([C:4]1[N:9]=[CH:8][C:7]([N:10]2[CH2:13][CH:12]([OH:14])[CH2:11]2)=[CH:6][CH:5]=1)([O-])=O>[Pd].C(O)C>[NH2:1][C:4]1[N:9]=[CH:8][C:7]([N:10]2[CH2:11][CH:12]([OH:14])[CH2:13]2)=[CH:6][CH:5]=1

참가 물질

4

반응물 1

HCID 592909581-(6-Nitro-pyridin-3-yl)-azetidin-3-ol

생성물 1

HCID 580438121-(6-Aminopyridin-3-yl)azetidin-3-ol수율 94%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A 100-mL single-neck round-bottomed flask was purged with nitrogen and charged with 147a (1.0 g, 5.1 mmol), 10% palladium on carbon (10% wet, 100 mg), and ethanol (40 mL). The mixture was evacuated, charged with hydrogen gas, and stirred at room temperature for 5 h. The hydrogen was then evacuated and nitrogen was charged into the flask. The catalyst was removed by filtration through a pad of CELITE® and the filtrate was concentrated under reduced pressure to afford 147b as a yellow solid (792 mg, 85%). MS-ESI: [M+H]+ 166.1.

후처리

  1. customA 100-mL single-neck round-bottomed flask was purged with nitrogen
  2. customThe mixture was evacuated
  3. additioncharged with hydrogen gas
  4. customThe hydrogen was then evacuated
  5. additionnitrogen was charged into the flask
  6. customThe catalyst was removed by filtration through a pad of CELITE®
  7. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1629b33d2f28403fa7d2d6bb66d1a26b
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754077B2

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