2,5-Dimethoxybenzoic acid → 5-Hydroxy-2-methoxybenzoic acid

HRID 446275

反応式

HRID 446275 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:9]([O:12]C)=[CH:8][C:4]=1[C:5]([OH:7])=[O:6]>S(=O)(=O)(O)O>[OH:12][C:9]1[CH:10]=[CH:11][C:3]([O:2][CH3:1])=[C:4]([CH:8]=1)[C:5]([OH:7])=[O:6]

参加物

3

実験手順

A solution of 2,5-dimethoxybenzoic acid (10.0 g, 54.9 mmol) in 55 mL concentrated sulfuric acid was heated to 55 deg. C. for 48 h. The reaction was then poured into ice. A precipitate formed, and the mixture was allowed to stand overnight. The resulting crystals were collected by filtration and dried in vacuo. The material was further purified by silica gel chromatography to give 5-hydroxy-2-methoxybenzoic acid as a white solid. MS m/z=169.0 [M+1]+. Calc'd for C8H8O4: 168.15.

後処理

  1. additionThe reaction was then poured into ice
  2. customA precipitate formed
  3. waitto stand overnight
  4. filtrationThe resulting crystals were collected by filtration
  5. customdried in vacuo
  6. customThe material was further purified by silica gel chromatography

出典と根拠

ORDレコード
ord-32f3ba746ca24d6a953da6c7c2b7a84f
出典データセット
uspto-grants-2013_07
特許番号
US08476434B2

関連ノート

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