2-Aminothiazole → HCID 67658626, compound

Temperature

80 °C

5 g (50 mmol) of 2-aminothiazole was dissolved in 15 ml of dimethylformamide, and 8.8 g (62.4 mmol) of 1-bromo-3-fluoropropane was added at room temperature. The reaction mixture was heated with stirring at 80° C. for 7.5 hours and then allowed to cool to room temperature. After addition of 300 ml of ethyl acetate, the reaction mixture was stirred at room temperature for 10 minutes. The resulting oily substance was separated from the ethyl acetate solution by decantation, and the same operation was repeated twice. The oily substance was crystallized by adding ethyl acetate and a small amount of methanol and filtered off to obtain 5.5 g of 2-imino-3-(3-fluoropropyl)thiazoline hydrobromide (4: Z=Br). Melting point 153°-155° C.

1. temperatureThe reaction mixture was heated
2. temperatureto cool to room temperature
3. stirringthe reaction mixture was stirred at room temperature for 10 minutes
4. customThe resulting oily substance was separated from the ethyl acetate solution by decantation
5. customThe oily substance was crystallized
6. additionby adding ethyl acetate
7. filtrationa small amount of methanol and filtered off

ORD record

ord-306ac54b46104d8c9f1c30e6639360ad

Source dataset

uspto-grants-1998_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05763365