反应详情

Intermediate 25 (216 mg, 1.083 mmol), intermediate 11 (198 mg, 0.903 mmol), HBTU (376 mg, 0.993 mmol) and triethylamine (377 μl, 2.71 mmol) were dissolved in dichloromethane (20 mL). The reaction mixture was stirred at room temperature for 14 hours. The reaction mixture was diluted with water and extracted with dichloromethane. The organic extract was washed with saturated ammonium chloride and dried over magnesium sulfate. The solution was concentrated in vacuo to give the crude material as a tan solid. The crude material was absorbed onto a plug of silica gel and purified by silica chromatography (hexane to ethyl acetate gradient) to provide N-(trans-3-(benzo[d]thiazol-2-ylamino)cyclobutyl)-2-(2-chloropyridin-3-yl)-2-methylpropanamide (220 mg, 0.549 mmol, 60.8% yield) as white solid.

1. extractionextracted with dichloromethane
2. extractionThe organic extract
3. washwas washed with saturated ammonium chloride
4. dry with materialdried over magnesium sulfate
5. concentrationThe solution was concentrated in vacuo
6. customto give the crude material as a tan solid
7. customThe crude material was absorbed onto a plug of silica gel
8. custompurified by silica chromatography (hexane to ethyl acetate gradient)