反应详情

温度

67.5 °C

A mixture of the product of Example 41E (7.50 g, 17.42 mmol) in 33% HBr in acetic acid (37 mL, 205.57 mmol, 11.8 equivalents) was heated to 65-70° C. for at least 6 hours while monitored by HPLC analysis for completion. When reaction is complete the mixture is cooled to not more than 45° C. and is diluted with methanol (111 mL). The mixture was cooled to 20-25° C., the product is collected by filtration and is washed with fresh methanol (50 mL). The wet cake is dried in the vacuum oven at not more than 55° C. to provide the title compound (7.25 g, 94.8%).

1. customWhen reaction
2. temperatureis cooled to not more than 45° C.
3. temperatureThe mixture was cooled to 20-25° C.
4. filtrationthe product is collected by filtration
5. washis washed with fresh methanol (50 mL)
6. customThe wet cake is dried in the vacuum oven at not more than 55° C.