Sodium Hydroxide → 3-[2,4-Dimethoxy-5-(4-methoxybenzoyl)phenyl]propionic acid

HRID 893418ノート

反応式

HRID 893418 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([C:11](=[O:20])[C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)=[CH:5][C:4]=1[CH2:21][CH2:22][C:23]([O:25]C)=[O:24].[OH-].[Na+]>O1CCOCC1>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([C:11](=[O:20])[C:12]2[CH:13]=[CH:14][C:15]([O:18][CH3:19])=[CH:16][CH:17]=2)=[CH:5][C:4]=1[CH2:21][CH2:22][C:23]([OH:25])=[O:24]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 14460995Methyl 3-[2,4-dimethoxy-5-(4-methoxybenzoyl)phenyl]propionate

生成物 1

HCID 144609963-[2,4-Dimethoxy-5-(4-methoxybenzoyl)phenyl]propionic acid

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

60.9 g of methyl 3-[2,4-dimethoxy-5-(4-methoxybenzoyl)phenyl]propionate are mixed with 300 ml of 2N sodium hydroxide solution and 300 ml of dioxane and stirred overnight. The dioxane is then removed in vacuo, and the alkaline aqueous solution is extracted once with 100 ml of ethyl acetate. The aqueous phase is adjusted to pH 2 with concentrated hydrochloric acid, when part of the product separates out. The mixture is extracted three times with 200 ml of ethyl acetate each time, and the organic phase is washed with water, dried over sodium sulfate and concentrated. The residue is recrystallized from ethyl acetate/acetone/hexane.

後処理

  1. customThe dioxane is then removed in vacuo
  2. extractionthe alkaline aqueous solution is extracted once with 100 ml of ethyl acetate
  3. extractionThe mixture is extracted three times with 200 ml of ethyl acetate each time
  4. washthe organic phase is washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue is recrystallized from ethyl acetate/acetone/hexane

出典と根拠

ORDレコード
ord-c243e0a9001f4ea59539d42c52d1062f
出典データセット
uspto-grants-1992_06
特許番号
US05124478

反応ノート

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