反应详情

The compound (909 mg) obtained in Example 129-2 was suspended in methanol (22 ml). Hydrazine monohydrate (0.13 ml) was dropped in this suspension. Then, the solution was subjected to thermal reflux for 4 hours. After completion of the reaction, the solvent was distilled off under reduced pressure and then the residue was subjected to extraction with chloroform. The organic layer was washed with water and then washed with saturated saline solution, followed by drying with anhydrous sodium sulfate. The residue obtained by distilling the solvent off was dissolved in DMF (15 ml) and added with triethylamine (0.54 ml) and di-t-butyl dicarbonate (851 mg), followed by stirring at room temperature for 15 hours. After the solvent had been distilled off, the residue was subjected to extraction with chloroform. The organic layer was washed with water and saturated saline solution and then dried with anhydrous sodium sulfate. The residue obtained by distilling the solvent off was purified through silica gel column chromatography (hexane/ethyl acetate), thereby obtaining the subject compound (779 mg) as a yellow oily substance.

1. temperaturethermal reflux for 4 hours
2. customAfter completion of the reaction
3. distillationthe solvent was distilled off under reduced pressure
4. extractionthe residue was subjected to extraction with chloroform
5. washThe organic layer was washed with water
6. washwashed with saturated saline solution
7. dry with materialby drying with anhydrous sodium sulfate
8. customThe residue obtained
9. distillationby distilling the solvent
10. dissolutionoff was dissolved in DMF (15 ml)
11. additionadded with triethylamine (0.54 ml) and di-t-butyl dicarbonate (851 mg)
12. distillationAfter the solvent had been distilled off
13. extractionthe residue was subjected to extraction with chloroform
14. washThe organic layer was washed with water and saturated saline solution
15. dry with materialdried with anhydrous sodium sulfate
16. customThe residue obtained
17. distillationby distilling the solvent
18. customoff was purified through silica gel column chromatography (hexane/ethyl acetate)