反应详情

To a mixture of the compound (1.6 g) obtained in Example 563, methylene chloride (20 ml) and triethylamine (0.92 ml), diphenylphosphorylazide (1.37 ml) was added. The reaction mixture was stirred at room temperature for 10 h and 2 N HCl and chloroform were added. The organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. To the resulting residue, water (16 ml) and 1,4-dioxane (32 ml) were added. The reaction mixture was heated under reflux for 2 h and 2 N HCl and chloroform were added. After adding 2 N aqueous sodium hydroxide solution and chloroform to the aqueous layer, the organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was recrystallized from a mixture of ethyl acetate and n-hexane to give 1.09 g of the titled compound (yield, 75%).

1. additionwas added
2. washThe organic layer was washed with a saturated aqueous sodium chloride solution
3. dry with materialdried with anhydrous sodium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. additionTo the resulting residue, water (16 ml) and 1,4-dioxane (32 ml) were added
6. temperatureThe reaction mixture was heated
7. temperatureunder reflux for 2 h
8. addition2 N HCl and chloroform were added
9. additionAfter adding 2 N aqueous sodium hydroxide solution and chloroform to the aqueous layer
10. washthe organic layer was washed with a saturated aqueous sodium chloride solution
11. dry with materialdried with anhydrous sodium sulfate
12. distillationthe solvent was distilled off under reduced pressure
13. customThe resulting residue was recrystallized from a mixture of ethyl acetate and n-hexane