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Sodium Hydroxide → HCID 70624201、化合物

HRID 2420093
ノート
印刷プレビュー

反応式

HRID 2420093 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[C:16]([OH:17])=[CH:15][CH:14]=[CH:13][N:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[OH-].[Na+]>O1CCOCC1.[Ni]>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C@H:11]2[C@@H:16]([OH:17])[CH2:15][CH2:14][CH2:13][NH:12]2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 43013592-(3,4-Dimethoxyphenyl)pyridin-3-ol

生成物 1

HCID 70624201HCID 70624201、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 312751,4-Dioxane溶媒

実験手順

2-(3,4-Dimethoxyphenyl)-3-pyridinol (10.0 g, 43.2 mmoles, described in Example 3) is dissolved in p-dioxane (60 ml) containing 0.1 ml of 12.5N sodium hydroxide. The solution is hydrogenated for 17 hours with Raney nickel catalyst (1.5 g) at 1750 p.s.i. and 140° C. The mixture is filtered and the filtrate is evaporated. The residue is subjected to chromatography on alumina (Woelm, basic activity I) using first chloroform as eluant and then a 1:10 methanol-chloroform solvent combination. The eluates are evaporated, dissolved in acetone and maleic acid is added. The precipitate is crystallized from isopropanol-hexane to give the title compound as the maleate salt, mp 180°-181° C.

後処理

  1. custom140° C
  2. filtrationThe mixture is filtered
  3. customthe filtrate is evaporated
  4. customThe eluates are evaporated
  5. dissolutiondissolved in acetone
  6. additionmaleic acid is added
  7. customThe precipitate is crystallized from isopropanol-hexane

出典と根拠

ORDレコード
ord-a0e932321ba548b79e6a6246ec185524
出典データセット
uspto-grants-1978_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04108997

反応ノート

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