Reaktion #648227

Reaktionsgleichung

7-chloro-3-(4-chloro-benzenesulfonyl)-quinolin-4-ol

phosphorus(V) oxybromide

sodium hydroxide

→

title compound

Ausbeute 77.0%

4-bromo-7-chloro-3-(4-chloro-benzenesulfonyl)-quinoline

Ausbeute 77.0%

Lösungsmittel

water

chloroform

triethylamine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for 6 hours
2. 2
   SonstigeThe organic layer was separated
3. 3
   Trocknendried over sodium sulfate
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated in vacuo
6. 6
   SonstigeThe obtained crude product
7. 7
   Sonstigewas purified by crystallization from diethyl ether

Vorschrift

A mixture of 7-chloro-3-(4-chloro-benzenesulfonyl)-quinolin-4-ol (0.5 g, 1.41 mmol) and phosphorus(V) oxybromide (1.2 g, 4.2 mmol) in chloroform (30 ml) and triethylamine (1 ml) was refluxed for 6 hours. The reaction mixture was diluted with water (30 ml) and the pH was adjusted to 10 with aqueous sodium hydroxide solution. The organic layer was separated, dried over sodium sulfate, filtered, and concentrated in vacuo. The obtained crude product was purified by crystallization from diethyl ether to obtain 0.45 g of the title compound in 77% yield.

Quelle