反応式
C([O:3][C:4](=[O:15])[C:5]([C:7]1[S:8][C:9]([Br:14])=[C:10]([Br:13])[C:11]=1[Br:12])=[O:6])C.Cl>CC(C)=O.O>[Br:12][C:11]1[C:10]([Br:13])=[C:9]([Br:14])[S:8][C:7]=1[C:5](=[O:6])[C:4]([OH:15])=[O:3]参加物
5
実験手順
A solution of (3,4,5-tribromothiophen-2-yl)-oxo-acetic acid ethyl ester (0.4 g, 0.95 mmol) in acetone (10 ml), water (2 ml), and conc. HCl (8 ml) was stirred under reflux for 1.5 hours. The reaction mixture was allowed to cool to ambient temperature and concentrated in vacuo to remove acetone which gave rise to solids which were collected, washed with water and dried. (3,4,5-tribromothiophen-2-yl)-oxo-acetic acid was thus obtained as a light yellow solid (0.17 g, 49%). MS (M−H)−: 392.75; 13C NMR (75 MHz, CDCl3) δ124.19, 117.80, 113.26, 111.72. IR (KBr) cm−1 3477.9, 3107.1, 2922.5, 1715.9, 1681.5, 1666.0, 1484.5, 1306.5, 1268.9.
後処理
- temperatureunder reflux for 1.5 hours
- concentrationconcentrated in vacuo
- customto remove acetone which
- customgave rise to solids which
- customwere collected
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-bd26dfa5677b41c5bf4baec1fcf716b3
- 出典データセット
- uspto-grants-2003_09
- 特許番号
- US06613786B2
関連ノート
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