反应详情

Thiophosgene (0.12 ml) and a solution of the compound (284 mg) obtained in Example 2 in methylene chloride (10 ml) were added dropwise to a suspension of calcium carbonate (319 mg) in water (5 ml) at room temperature and stirred at room temperature for 5 h; thereafter, a 28% aqueous ammonia solution (5 ml) was added to the reaction mixture and stirred at room temperature for 16 h. After neutralization with 2 N HCl, the reaction mixture was extracted with ethyl acetate and the organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=6:4) to yield 351 mg of the titled compound (yield, 89%).

1. stirringstirred at room temperature for 16 h
2. extractionAfter neutralization with 2 N HCl, the reaction mixture was extracted with ethyl acetate
3. washthe organic layer was washed with a saturated aqueous sodium chloride solution
4. dry with materialdried with anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=6:4)