反应详情

In 66 ml of dimethyl sulfoxide was dissolved 13.2 g of ethyl 3-difluoromethoxy-2,4,5-trifluorobenzoate, and to this solution was added 7.3 g of sodium azide, after which the resulting mixture was stirred at room temperature for five hours. The reaction mixture was added to a mixed solvent of 150 ml of ethyl acetate and 150 ml of ice water and the pH was adjusted to 2 with 6N hydrochloric acid, after which the organic layer formed was separated, then washed successively with water and a saturated saline solution, and thereafter dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure. The residue obtained was purified by a column chromatography (eluent: n-hexane:ethyl acetate=10:1), to obtain 13.9 g of colorless, oily ethyl 4-azido-2,5-difluoro-3-difluorome-thoxybenzoate.

1. customafter which the organic layer formed
2. customwas separated
3. washwashed successively with water
4. dry with materiala saturated saline solution, and thereafter dried over anhydrous magnesium sulfate
5. customThe solvent was then removed by distillation under reduced pressure
6. customThe residue obtained
7. customwas purified by a column chromatography (eluent: n-hexane:ethyl acetate=10:1)