反应详情

4.85 g (17.46) mmol of the compound of Example 12A were dissolved in 17 ml (52.39 mmol) of 3M aqueous sodium hydroxide solution and heated under reflux for 168 h. After 16, 40, 64 and 88 h, in each case 1.05 g (26.19 mmol, 104.76 mmol in total) of solid sodium hydroxide were added. Using 1M hydrochloric acid, the mixture was adjusted to pH 10, and the mixture was extracted twice with in each case 30 ml of ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered, freed from the solvent on a rotary evaporator and dried under high vacuum. This gave 2.44 g (54% of theory) of the title compound.

1. temperatureheated
2. temperatureunder reflux for 168 h
3. extractionthe mixture was extracted twice with in each case 30 ml of ethyl acetate
4. dry with materialThe combined organic phases were dried over sodium sulphate
5. filtrationfiltered
6. customfreed from the solvent on a rotary evaporator
7. customdried under high vacuum