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

HRID 407770ノート

反応式

HRID 407770 の反応式
[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

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1629b33d2f28403fa7d2d6bb66d1a26b
出典データセット
uspto-grants-2014_06
特許番号
US08754077B2

反応ノート

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