(+/-)-(E)-1-(4-(2-Phenylethenyl)phenoxy)-4-(3-pyridyl)-2-butanol → HCID 21830747、化合物

HRID 1600950ノート

反応式

HRID 1600950 の反応式
[C:1]1(/[CH:7]=[CH:8]/[C:9]2[CH:26]=[CH:25][C:12]([O:13][CH2:14][CH:15]([OH:24])[CH2:16][CH2:17][C:18]3[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=3)=[CH:11][CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>C(O)C.[Pd]>[C:1]1([CH2:7][CH2:8][C:9]2[CH:26]=[CH:25][C:12]([O:13][CH2:14][CH:15]([OH:24])[CH2:16][CH2:17][C:18]3[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=3)=[CH:11][CH:10]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 1

HCID 21830666(+/-)-(E)-1-(4-(2-Phenylethenyl)phenoxy)-4-(3-pyridyl)-2-butanol

生成物 1

HCID 21830747HCID 21830747、化合物収率 90.1%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A solution of (±)-(E)-1-(4-(2-phenylethenyl)phenoxy)-4-(3-pyridyl)-2-butanol (0.32 g, Example 61) was dissolved in dry ethanol (50 ml) and hydrogenated for 24 hours at 3 atmospheres using palladium on carbon (10%, 0.1 g) as catalyst. The reaction mixture was filtered through Celite® and the residue washed with ethanol. The filtrate and washings were combined and concentrated under reduced pressure. The residue was purified by column chromatography over silica eluting with dichloromethane:methanol (95:5) to give the title compound as a white solid (0.29 g).

後処理

  1. filtrationThe reaction mixture was filtered through Celite®
  2. washthe residue washed with ethanol
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by column chromatography over silica eluting with dichloromethane:methanol (95:5)

出典と根拠

ORDレコード
ord-e4579a396d494de1bd441c88e9e8c030
出典データセット
uspto-grants-1999_11
特許番号
US05977105

反応ノート

読み込み中…