Sulfuric Acid → HCID 608316、化合物
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH:16](O)([CH3:18])[CH3:17]>O>[CH:16]([O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][CH:10]=[C:2]([Br:1])[CH:3]=1)([CH3:18])[CH3:17]参加物
5
実験手順
A solution of 3-bromo benzoic acid (Aldrich, 2.4 g, 11.9 mmol) in isopropanol (20 mL) was treated with 1 mL of concentrated sulfuric acid and the resulting reaction mixture was refluxed overnight. The reaction mixture was then cooled to ambient temperature and diluted with water and extracted with diethyl ether. The organic phase was dried over anhydrous sodium sulfate, filtered and evaporated to an oil that was subjected to flash column chromatography over silica gel (230-400 mesh) using 10% ethyl acetate in hexane as the eluent to afford the title compound as an oil (2.54 g, 88%).
後処理
- customthe resulting reaction mixture
- temperaturewas refluxed overnight
- extractionextracted with diethyl ether
- dry with materialThe organic phase was dried over anhydrous sodium sulfate
- filtrationfiltered
- customevaporated to an oil that
出典と根拠
- ORDレコード
- ord-02738807d9c140879264d979d9867ab4
- 出典データセット
- uspto-grants-2009_12
- 特許番号
- US07638648B2
反応ノート
読み込み中…