Reaktion #466125

Reaktionsgleichung

sodium acetate

7-chloro-5-(4-fluorophenyl)thieno[3,2-b]pyridine

4-(1H-imidazol-2-yl)piperidine. hydrochloride

→

5-(4-fluorophenyl)-7-(4-imidazol-2-ylpiperidyl)thiopheno[3,2-b]pyridine

Ausbeute 18.0%

Lösungsmittel

ethylene glycol

ethylacetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturIt is then cooled
2. 2
   Waschenwashed with water (3×15 mL)
3. 3
   TrocknenThe organic layer is dried over sodium sulfate
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated
6. 6
   SonstigeThe residue is purified by preparative thin layer chromatography

Vorschrift

A mixture of 7-chloro-5-(4-fluorophenyl)thieno[3,2-b]pyridine (146 mg, 0.53 mmol), 4-(1H-imidazol-2-yl)piperidine. hydrochloride (U.S. Pat. No. 4,431,653) (100 mg, 0.53 mmole) and sodium acetate (50 mg) in ethylene glycol (10 mL) is stirred and heated at 160° C. for about 16 hours. It is then cooled, diluted with ethylacetate (15 mL), and washed with water (3×15 mL). The organic layer is dried over sodium sulfate, filtered, and concentrated. The residue is purified by preparative thin layer chromatography to give 5-(4-fluorophenyl)-7-(4-imidazol-2-ylpiperidyl)thiopheno[3,2-b]pyridine (36 mg, 18% yield) as a white solid, m.p. 95° C. (compound 1).

Quelle