反应详情

温度

80 °C

To a solution of 4-cyclopropyl benzoic acid (0.58 g, 3.57 mmol) in toluene (2 ml), thionyl chloride (1.29 ml, 17.87 mmol) was added. The mixture was stirred at 80° C. for 2 hours and afterwards evaporated under reduced pressure. The residue was dissolved together with Intermediate 20 (1.0 g, 2.36 mmol) in pyridine (5 ml) and the mixture was stirred at room temperature for 2 hours. Pyridine was evaporated under reduced pressure and the residue was dissolved in DCM and washed with saturated sodium hydrogen carbonate solution and brine (2×). The residue was purified by flash chromatography on silica (cyclohexane to EtOAc) to afford the compound Intermediate 21 as a beige solid.

1. customafterwards evaporated under reduced pressure
2. stirringthe mixture was stirred at room temperature for 2 hours
3. customPyridine was evaporated under reduced pressure
4. dissolutionthe residue was dissolved in DCM
5. washwashed with saturated sodium hydrogen carbonate solution and brine (2×)
6. customThe residue was purified by flash chromatography on silica (cyclohexane to EtOAc)