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2-((4-Methoxybenzyl)amino)isonicotinonitrile → (4-Aminomethyl-pyridin-2-yl)-(4-methoxy-benzyl)-amine

HRID 887634
ノート
印刷プレビュー

反応式

HRID 887634 の反応式
[CH3:1][O:2][C:3]1[CH:18]=[CH:17][C:6]([CH2:7][NH:8][C:9]2[CH:10]=[C:11]([CH:14]=[CH:15][N:16]=2)[C:12]#[N:13])=[CH:5][CH:4]=1>CCO.[Pd]>[NH2:13][CH2:12][C:11]1[CH:14]=[CH:15][N:16]=[C:9]([NH:8][CH2:7][C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:18][CH:17]=2)[CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 219613782-((4-Methoxybenzyl)amino)isonicotinonitrile

生成物 1

HCID 21961478(4-Aminomethyl-pyridin-2-yl)-(4-methoxy-benzyl)-amine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

2-(4-Methoxy-benzylamino)-isonicotinonitrile (12 g, 50 mmole) was dissolved in a mixed solvent of EtOH (800 mL) Et3N (200 mL) and suspended with 2 g of Pd/C (10%). After removing air with vacuum, the flask was charged with H2 with a balloon. The H2 balloon was refilled every morning and evening. Pd/C was recharged twice (1.3 g each) on days 2 and 3. Reaction was completed on the 4th day and the reaction mixture was filtered through a pad of Celite®. The filter cake was rinsed with MeOH and the combined filtrate was concentrated in vacuo to give the desired compound as a light brown solid.

後処理

  1. customAfter removing air with vacuum
  2. additionthe flask was charged with H2 with a balloon
  3. additionThe H2 balloon was refilled every morning and evening
  4. customReaction
  5. filtrationthe reaction mixture was filtered through a pad of Celite®
  6. washThe filter cake was rinsed with MeOH
  7. concentrationthe combined filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-28cf3d4ae8ea48e7a6500c3a847b8a86
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08247430B2

反応ノート

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