Hydrochloric Acid → HCID 22997662, Verbindung

HRID 1166212

Reaktionsgleichung

Reaktionsgleichung von HRID 1166212
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]

Komponenten

5

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-bd26dfa5677b41c5bf4baec1fcf716b3
Quelldatensatz
uspto-grants-2003_09
Patentnummer
US06613786B2

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