反应详情

温度

10 °C

To 3.02 g (10.3 mmol) of the above-obtained 2-(N-methyl-N-trifluoroacetylaminomethylcarbonyl)aminomethylthiazole was added 40 ml of phosphorus oxychloride, and the mixture was stirred at 10° C. for 1.5 hours and then at 120° C. for 5 hours. The reaction solution was cooled to room temperature, and concentrated under reduced pressure. To the residue were added a small amount of ice and 15 ml of a 50% aqueous solution of potassium carbonate. The mixture was stirred, and then extracted three times with methylene chloride. The organic layer was dried over anhydrous potassium carbonate, concentrated under reduced pressure, and purified by flash column chromatography using silica gel, eluting with a 1:9 mixture of hexane and ethyl acetate to give 490 mg (yield 18%) of 5-(N-methyl-N-trifluoroacetylamino)methylimidazo[5,1-b]thiazole as colorless crystals.

1. waitat 120° C. for 5 hours
2. temperatureThe reaction solution was cooled to room temperature
3. concentrationconcentrated under reduced pressure
4. additionTo the residue were added a small amount of ice and 15 ml of a 50% aqueous solution of potassium carbonate
5. stirringThe mixture was stirred
6. extractionextracted three times with methylene chloride
7. dry with materialThe organic layer was dried over anhydrous potassium carbonate
8. concentrationconcentrated under reduced pressure
9. custompurified by flash column chromatography
10. washeluting with a 1:9 mixture of hexane and ethyl acetate