HCID 22916669, compound → HCID 22916686, compound

Temperature

100 °C

To 1.98 g of the above-obtained 2-[(N-trifluoroacetylglycyl)amino]methylthiazole was added 20 ml of phosphorus oxychloride, and the mixture was heated and stirred at 100° C. for 4.5 hours. The reaction solution was cooled to room temperature, and concentrated to dryness under reduced pressure. The residue was dissolved in 30 ml of methylene chloride. To this solution was added 50 ml of water with ice- cooling. The pH of the mixture was adjusted to 8 by adding potassium carbonate little by little with ice-cooling, and the mixture was stirred for one hour. The crystals precipitated were collected by filtration, washed with cold water and a small amount of cold methylene chloride, and dried under reduced pressure to give 1.12 g (yield 60%) of 5-(trifluoro- acetylamino)methylimidazo[5,1-b]thiazole as light yellow crystals.

1. temperaturethe mixture was heated
2. temperatureThe reaction solution was cooled to room temperature
3. concentrationconcentrated to dryness under reduced pressure
4. dissolutionThe residue was dissolved in 30 ml of methylene chloride
5. additionTo this solution was added 50 ml of water with ice-
6. temperaturecooling
7. additionby adding potassium carbonate little by little with ice-
8. temperaturecooling
9. stirringthe mixture was stirred for one hour
10. customThe crystals precipitated
11. filtrationwere collected by filtration
12. washwashed with cold water
13. dry with materiala small amount of cold methylene chloride, and dried under reduced pressure

ORD record

ord-f81bff87d88042f083693946477116b0

Source dataset

uspto-grants-1997_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05663162