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2-Bromo-5-fluoro-4-((1-methylpiperidin-4-yl)oxy)-3-nitropyridine → 5-Fluoro-4-((1-methylpiperidin-4-yl)oxy)pyridin-3-amine

HRID 524939
ノート
印刷プレビュー

反応式

HRID 524939 の反応式
Br[C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([O:11][CH:12]2[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]2)[C:5]([F:19])=[CH:4][N:3]=1.[H][H]>CO.[Zn+2].[Br-].[Br-].[Pd]>[F:19][C:5]1[C:6]([O:11][CH:12]2[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]2)=[C:7]([NH2:8])[CH:2]=[N:3][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 867209972-Bromo-5-fluoro-4-((1-methylpiperidin-4-yl)oxy)-3-nitropyridineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 867209985-Fluoro-4-((1-methylpiperidin-4-yl)oxy)pyridin-3-amine

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 10421208Zinc bromide触媒HCID 887Methanol
溶媒

実験手順

A solution of 2-bromo-5-fluoro-4-[(1-methyl-4-piperidyl)oxy]-3-nitro-pyridine (96 mg, 0.2873 mmol), ZnBr2 (12.94 mg, 3.080 μL, 0.05746 mmol) and Pd on C, wet, Degussa (31 mg) in methanol (5 mL) was flushed with hydrogen and evacuated (3×) and then stirred under a hydrogen atmosphere overnight. The catalyst was filtered off through a celite pad and washed with methanol and ethyl acetate mixtures and the filtrate was concentrated in vacuo to leave a pale yellow oil that was used in next step without further purification. MS (ES+) 226.1.

後処理

  1. customevacuated (3×)
  2. filtrationThe catalyst was filtered off through a celite pad
  3. washwashed with methanol and ethyl acetate mixtures
  4. concentrationthe filtrate was concentrated in vacuo
  5. customto leave a pale yellow oil that
  6. customwas used in next step without further purification

出典と根拠

ORDレコード
ord-8ba64bcbe6fe43dc9ebedbeb7598ba9b
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09340546B2

反応ノート

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