HCID 23103640、化合物 → 4-(4-Ethylbenzyl)-3-hydroxypyridine

HRID 2116484ノート

反応式

HRID 2116484 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]([C:11]2[CH:16]=[CH:15][N:14]=[CH:13][C:12]=2[OH:17])O)=[CH:5][CH:4]=1)[CH3:2]>[Pd].C(O)(=O)C>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:11]2[CH:16]=[CH:15][N:14]=[CH:13][C:12]=2[OH:17])=[CH:5][CH:4]=1)[CH3:2]

参加物

4

反応物 1

HCID 23103640HCID 23103640、化合物

生成物 1

HCID 231036434-(4-Ethylbenzyl)-3-hydroxypyridine収率 40%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

Next, to a mixture of (4-ethylphenyl)-(3-hydroxypyridin-4-yl)-methanol (10.54 g, 46.0 mmol) and acetic acid (100 ml), 5% palladium/carbon (5.0 g) was added and stirred under a hydrogen atmosphere at room temperature for 7 hours. After filtration to remove the insoluble materials, the filtrate was concentrated under reduced pressure and the resulting residue was recrystallized (ethyl acetate) to give the titled compound (3.91 g, 40%) as a colorless powder. Moreover, the mother liquor was purified by NH silica gel column chromatography (chloroform:methanol=20:1) to give 4-(4-ethylbenzyl)-3-hydroxypyridine (4.55 g, 46%) as a light-brown powder.

後処理

  1. additionwas added
  2. filtrationAfter filtration
  3. customto remove the insoluble materials
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customthe resulting residue was recrystallized (ethyl acetate)

出典と根拠

ORDレコード
ord-1bf123a11d6440c39ae6436454dcd890
出典データセット
uspto-grants-2008_10
特許番号
US07439232B2

反応ノート

読み込み中…