Reaktion #1435732

Reaktionsgleichung

5-hydroxy-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine

N,N-diethylaniline

phosphorus oxychloride

→

5-chloro-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed
2. 2
   Temperaturunder heating for 26 hours
3. 3
   EinengenThe reaction mixture was concentrated
4. 4
   workup.ADDITIONdichloromethane and aqueous saturated sodium bicarbonate solution were added to the residue
5. 5
   WaschenThe separated organic layer was washed with water
6. 6
   Trocknendried over sodium sulfate
7. 7
   Einengenconcentrated

Vorschrift

A mixture of 0.16 g of 5-hydroxy-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine, 0.20 g of N,N-diethylaniline and 2 ml of phosphorus oxychloride was refluxed under heating for 26 hours. The reaction mixture was concentrated, and dichloromethane and aqueous saturated sodium bicarbonate solution were added to the residue. The separated organic layer was washed with water, dried over sodium sulfate and concentrated. The residue was subjected to silica gel chromatography to give 45mg of 5-chloro-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine.

Quelle