反应详情

Potassium carbonate (0.2 g) is suspended in a solution of [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 20, Step D) (0.4 g, 0.0011 mole) in dimethylformamide (3 ml). After warming the suspension on a steam bath for 15 minutes, chloroacetone (0.5 g, 0.005 mole) is added and the mixture heated for an additional 15 minutes. The reaction mixture is cooled, poured into water (50 ml) and the product extracted into ether (three 15 ml portions. The extract is dried over Na2SO4. After filtration, the extract is concentrated to give a yellow oil. Trituration with cold ether causes crystallization to occur. The crystalline product weighs 0.1 g and melts at 153°-155° C.

1. temperatureAfter warming the suspension on a steam bath for 15 minutes
2. temperaturethe mixture heated for an additional 15 minutes
3. temperatureThe reaction mixture is cooled
4. extractionthe product extracted into ether (three 15 ml portions
5. dry with materialThe extract is dried over Na2SO4
6. filtrationAfter filtration
7. concentrationthe extract is concentrated
8. customto give a yellow oil
9. customcrystallization