反应详情

温度

85 °C

A mixture of 5-(4-fluoro-benzyl)-thiazol-2-ylamine (330 mg, 1.59 mmol) and 2-bromoethyl methyl ether (0.50 mL, 5.34 mmol) was heated to 85° C. and stirred for 12 hours. The mixture was cooled to ambient temperature, diluted with 20 mL of ethyl acetate and washed with saturated aqueous NaHCO3. The layers were separated and the aqueous phase was extracted with 2×20 mL ethyl acetate and the combined organic extracts were dried over anhydrous Na2SO4, filtered, and concentrated. Purification by column chromatography (SiO2, 50% ethyl acetate in dichloromethane containing 0.5% Et3N) afforded 342 mg of the title compound: MS (LC/MS) m/z 267 (M+H)+.

1. temperatureThe mixture was cooled to ambient temperature
2. washwashed with saturated aqueous NaHCO3
3. customThe layers were separated
4. extractionthe aqueous phase was extracted with 2×20 mL ethyl acetate
5. dry with materialthe combined organic extracts were dried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification by column chromatography (SiO2, 50% ethyl acetate in dichloromethane containing 0.5% Et3N)