反应详情

温度

70 °C

N-{5-[(3-Amino-4-fluorophenyl)amino][1,3]thiazolo[5,4-b]pyridin-2-yl}cyclopropanecarboxamide (200 mg, 0.58 mmol) produced in Example 12(v) was dissolved in pyridine (3.0 mL), 1-chloro-4-isocyanato-2-(trifluoromethyl)benzene (190 mg, 0.88 mmol) was added, and the mixture was stirred at 70° C. for 8 hr. The reaction mixture was cooled to room temperature, diluted with ethyl acetate (10 mL), and washed successively with water (10 mL) and saturated brine (10 ml). The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The obtained residue was purified by basic silica gel column chromatography (ethyl acetate/hexane=10/90→80/20), and the obtained solution was concentrated under reduced pressure. The residue was recrystallized from ethyl acetate to give the title compound (130 mg, 39%) as a colorless powder.

1. temperatureThe reaction mixture was cooled to room temperature
2. washwashed successively with water (10 mL) and saturated brine (10 ml)
3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe obtained residue was purified by basic silica gel column chromatography (ethyl acetate/hexane=10/90→80/20)
6. concentrationthe obtained solution was concentrated under reduced pressure
7. customThe residue was recrystallized from ethyl acetate