反应详情

Intermediate 1 (1.75 g, 7.32 mmol) was dissolved in glacial acetic acid (30 ml) and then treated with concentrated sulfuric acid (0.8 ml) followed by water (2.8 ml) with stirring. This mixture was then treated with periodic acid (0.23 eq., 0.38 g, 1.67 mmol) then iodine (0.43 eq., 800 mg, 3.15 mmol), and the whole mix was stirred at 60° C. for 3-4 h. The reaction mixture was allowed to cool and then partitioned between ethyl acetate and 10% aqueous sodium metabisulfite. The organic layer was separated and dried over sodium sulphate and evaporated in vacuo to give the title compound as a yellow oil (2.95 g).

1. stirringwas stirred at 60° C. for 3-4 h
2. temperatureto cool
3. custompartitioned between ethyl acetate and 10% aqueous sodium metabisulfite
4. customThe organic layer was separated
5. dry with materialdried over sodium sulphate
6. customevaporated in vacuo