反应详情

温度

90 °C

A solution of N-(4-(3-bromopyridin-2-yloxy)phenyl)benzo[d]thiazol-2-amine (600 mg, 1.506 mmol), 2-cyclopenten-1-one (0.609 mL, 7.53 mmol), n-methyldicyclohexylamine (0.959 mL, 4.52 mmol) and bis(tri-tert-butylphosphine)palladium (0) (77 mg, 0.151 mmol) in Dioxane (4 mL) was capped, degassed and backfilled with argon. The reaction was heated to 90° C. After 6 h, the reaction was heated to 110° C. After 36 h, the reaction was cooled to 23° C., diluted with EtOAc (150 mL) and washed with water (100 mL) and brine (100 mL), dried over MgSO4, concentrated in vacuo and purified by silica gel chromatography (eluant: 0.5-3% methanol/dichloromethane), affording the product as a yellow solid. MS (ESI, pos. ion) m/z: 400.1 (M+1).

1. customdegassed
2. temperaturethe reaction was heated to 110° C
3. waitAfter 36 h
4. temperaturethe reaction was cooled to 23° C.
5. additiondiluted with EtOAc (150 mL)
6. washwashed with water (100 mL) and brine (100 mL)
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo
9. custompurified by silica gel chromatography (eluant: 0.5-3% methanol/dichloromethane)