反应详情

The compound obtained in Example 66-3 (8.96 g) was dissolved in methanol (134.4 ml) and 1 N aqueous solution of sodium hydroxide (134.4 ml) was added. The mixture was stirred for 1 day. After confirming completion of the reaction with TLC, the reaction solution was concentrated under reduced pressure. The residue was dissolved in 1N aqueous solution of sodium hydroxide and washed with diisopropyl ether. 1 N hydrochloric acid aqueous solution was added to the resulting water layer to adjust the pH to 2-3. The solution was extracted with ethyl acetate and the organic layer separated was dried over anhydrous sodium sulfate, concentrated under reduced pressure, and dried under vacuum to obtain the title compound (8.04 g) as a light brown solid.

1. customcompletion of the reaction with TLC
2. concentrationthe reaction solution was concentrated under reduced pressure
3. dissolutionThe residue was dissolved in 1N aqueous solution of sodium hydroxide
4. washwashed with diisopropyl ether
5. addition1 N hydrochloric acid aqueous solution was added to the resulting water layer
6. extractionThe solution was extracted with ethyl acetate
7. customthe organic layer separated
8. dry with materialwas dried over anhydrous sodium sulfate
9. concentrationconcentrated under reduced pressure
10. customdried under vacuum