Hydrochloric Acid → HCID 22997662、化合物

HRID 1166212

反応式

HRID 1166212 の反応式
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

  1. temperatureunder reflux for 1.5 hours
  2. concentrationconcentrated in vacuo
  3. customto remove acetone which
  4. customgave rise to solids which
  5. customwere collected
  6. washwashed with water
  7. 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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