反应详情

温度

5 °C

A mixture of 1B (2.38 g) and methanol (20 ml) was added to a stirred solution of sodium hydroxide (1.68 g) in water (20 ml). The reaction mixture was heated at reflux for 3 hours. The reaction mixture was cooled to roomtempeature and concentrated in vacuo. The concentrate was cooled to 5° C. and acidified with concentrated HCl (3.5 ml). The resulting suspension was stirred at 5° C. for 30 minutes. The solid was collected by filtration, washed with water, then dried in vacuo at 35-40° C. to give the free acid (1.45 g, 65%).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 3 hours
3. temperatureThe reaction mixture was cooled to roomtempeature
4. concentrationconcentrated in vacuo
5. filtrationThe solid was collected by filtration
6. washwashed with water
7. customdried in vacuo at 35-40° C.