Reaktion #1606205

Reaktionsgleichung

2-chloro-5-chloromethylpyridine

acetonitrile

potassium carbonate

1,1,1-trifluoro-3-(thiaolidin-2-ylidene)propane-2-one

→

target compound

Ausbeute 50.0%

3-[3-((6-chloropyridin-3-yl)methyl)thiazolidin-2-ylidene]-1,1,1-trifluoropropan-2-one

Ausbeute 50.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeobtained by the foregoing method
2. 2
   Temperaturthe mixture was refluxed
3. 3
   Temperaturunder heating for 2 hours
4. 4
   SonstigeAfter reaction completion
5. 5
   Sonstigewas returned to room temperature
6. 6
   Sonstigeinsoluble matter was removed by filtration
7. 7
   Einengenthe filtrate was concentrated under reduced pressure
8. 8
   SonstigeThe concentrate was purified by silica gel column chromatography (hexane/ethyl acetate=1:1→1:3)

Vorschrift

2-chloro-5-chloromethylpyridine (80 mg, 0.50 mmol) dissolved in 8 mL of anhydrous acetonitrile, and potassium carbonate (69 mg, 0.50 mmol) were added to 65 mg (0.33 mmol) of 1,1,1-trifluoro-3-(thiaolidin-2-ylidene)propane-2-one obtained by the foregoing method, and the mixture was refluxed under heating for 2 hours. After reaction completion, the reaction mixture was returned to room temperature, insoluble matter was removed by filtration, and the filtrate was concentrated under reduced pressure. The concentrate was purified by silica gel column chromatography (hexane/ethyl acetate=1:1→1:3), giving 53 mg of the target compound (yield, 50%).

Quelle