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温度

0 °C

Ethyl {4-[4,9-bis(ethyloxy)-1-hydroxy-3-oxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl]-2-fluorophenyl}acetate (approx. 51.6 mmol) was dissolved in CH2Cl2 (50 ml) and cooled to 0° C. and TFA (50 ml) added. Triethylsilane (12.3 ml, 77 mmol) was added in one portion to give a brown solution. The solution was concentrated in vacuo to give a tan solid. This was recrystallised from hot isopropanol (550 ml), cooled, filtered, washed with isopropanol, and dried in a vacuum oven to give the title compound as off white crystals (20.2 g).

1. customto give a brown solution
2. concentrationThe solution was concentrated in vacuo
3. customto give a tan solid
4. customThis was recrystallised from hot isopropanol (550 ml)
5. temperaturecooled
6. filtrationfiltered
7. washwashed with isopropanol
8. customdried in a vacuum oven