反应详情

Compound 2b (80 mg) was dissolved in ethanol (2.6 ml), and a 2N sodium hydroxide aqueous solution (1.7 ml) was added to the obtained solution in a nitrogen atmosphere. The mixture was stirred overnight at room temperature. A 2N hydrochloric acid aqueous solution (3.4 ml) was added thereto. The resulting white precipitate was filtered off and dissolved in ethyl acetate. The reaction mixture was separated with ethyl acetate and water. The organic layer was washed with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate. After the solvent was distilled off and n-hexane was added to the obtained residue, the mixture was pulverized with ultrasonic waves. The solid was filtered off, and the obtained powder was dissolved in butyl acetate (0.5 ml) by heating. The reaction mixture was allowed to cool and then filtered. Thus, Compound 2 (39 mg, 55%) was obtained as an opalescent solid.

1. filtrationThe resulting white precipitate was filtered off
2. dissolutiondissolved in ethyl acetate
3. customThe reaction mixture was separated with ethyl acetate and water
4. washThe organic layer was washed with a saturated sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationAfter the solvent was distilled off
7. additionn-hexane was added to the obtained residue
8. filtrationThe solid was filtered off
9. dissolutionthe obtained powder was dissolved in butyl acetate (0.5 ml)
10. temperatureby heating
11. temperatureto cool
12. filtrationfiltered