反应详情

The compound (909 mg) obtained in Example 7-2 was suspended in methanol (22 ml). Hydrazine monohydrate (0.13 ml) was dropped in this suspension and the whole was refluxed under heating 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 with a 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-butyldicarbonate (851 mg), followed by stirring at room temperature for 15 hours. After the solvent was distilled off, the residue was subjected to extraction with chloroform. The organic layer was washed with water and a 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. temperaturethe whole was refluxed
2. temperatureunder heating for 4 hours
3. customAfter completion of the reaction
4. distillationthe solvent was distilled off under reduced pressure
5. extractionthe residue was subjected to extraction with chloroform
6. washThe organic layer was washed with water
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-butyldicarbonate (851 mg)
12. distillationAfter the solvent was distilled off
13. extractionthe residue was subjected to extraction with chloroform
14. washThe organic layer was washed with water
15. dry with materiala saturated saline solution and then dried 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)