反应详情

温度

0 °C

A suspension of ethyl {-4-[4,9-bis(ethyloxy)-1-oxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl]-2-fluorophenyl}acetate (200.0 g, 443 mmol) in a mixture of glacial acetic acid (2080 mL) and hydrochloric acid (2 M, 700 mL) was heated to reflux under a nitrogen atmosphere, with the reaction progress monitored by TLC analysis (silica, dichloromethane:methanol, 99:1). After 60 minutes the reaction mixture was cooled to 0° C. The precipitated solid was isolated by filtration, washed with water (1400 mL), and freeze-dried to give the desired product as an off-white solid (163.4 g, 87% yield).

1. temperaturewas heated
2. temperatureto reflux under a nitrogen atmosphere, with the reaction progress
3. customThe precipitated solid was isolated by filtration
4. washwashed with water (1400 mL)
5. customfreeze-dried