反应详情

A mixture of 19 (158 g, 0.7 mol) and acetic acid (700 mL) was heated under reflux for 5 hrs. The reaction mixture was cooled to room temperature, the precipitate filtered and the bright yellow filter cake washed with water (5×500 mL). The filter cake was recrystallized from ethyl acetate (200 mL), filtered and dried over a medium frit sintered glass funnel in vacuo to give the desired product 20 in 32% yields. HPLC (tr/purity): 15.37 min, >95%. ESI m/z (MeOH): 2073 (MH+).

1. temperaturewas heated
2. temperatureunder reflux for 5 hrs
3. filtrationthe precipitate filtered
4. washthe bright yellow filter cake washed with water (5×500 mL)
5. customThe filter cake was recrystallized from ethyl acetate (200 mL)
6. filtrationfiltered
7. customdried over a medium frit sintered glass funnel in vacuo