反应详情

温度

100 °C

Ethyl 2-bromo-2-phenylacetate (0.28 ml, 1.64 mmol), ortho-toluidine (0.26 ml, 2.47 mmol), and DIPEA (0.43 ml, 2.47 mmol) were dissolved in acetonitrile (5 ml) and stirred under microwave irradiation at 100° C. for 1 hours (Conversion complete by UPLC/MS-UV). Lithium hydroxide hydrate (207 mg, 4.94 mmol) and water (3 ml) were added, and the mixture was stirred at room temperature for 16 hours. 4M HCl in dioxane was added until pH was about 1, then the solvents were evaporated, the residue was suspended in water, sonicated, and cooled at 0° C., and the resulting solid was recovered by filtration and dried under vacuum to get intermediate I22 (290 mg, 63% yield).

1. stirringthe mixture was stirred at room temperature for 16 hours
2. customthe solvents were evaporated
3. customsonicated
4. temperaturecooled at 0° C.
5. filtrationthe resulting solid was recovered by filtration
6. customdried under vacuum
7. customto get intermediate I22 (290 mg, 63% yield)