Reaktion #45426

Reaktionsgleichung

solution

3-bromo-7-methylthieno[3,2-c]pyridin-4(5H)-one

POCl3

→

desired product

Ausbeute 64.0%

3-bromo-4-chloro-7-methylthieno[3,2-c]pyridine

Ausbeute 64.0%

Lösungsmittel

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 2 hours
2. 2
   Sonstigeresulting in a precipitate which
3. 3
   Filtrationwas collected by filtration
4. 4
   SonstigeThe filter cake was further purified by silica gel chromatography on silica gel with dichloromethane

Vorschrift

A solution of Example 277B (10,25 g, 42.1 mmol) in POCl3 (50 mL) was stirred at reflux for 2 hours, cooled to room temperature, diluted with ice water, and stirred vigorously resulting in a precipitate which was collected by filtration. The filter cake was further purified by silica gel chromatography on silica gel with dichloromethane to provide 7.14 g (64% yield) of the desired product. MS (ESI(+)) m/e 261.9, 263.9 (M+H)+.

Quelle