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
- additionThe reaction was then poured into ice
- customA precipitate formed
- waitto stand overnight
- filtrationThe resulting crystals were collected by filtration
- customdried in vacuo
- 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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