反应详情

A solution of the product of Step 2 (15 g) in 70 mL of MeOH and 50 mL of CH2Cl2 was treated with a stream of ozone/oxygen until the solution turned light blue. Dimethylsulfide (20 mL) was added and the reaction mixture was stirred for 2 h at room temperature and then treated with 5 g of triphenylphosphine for an additional 0.5 h. DBU (1 mL) was then added to the reaction mixture. After stirring for 1 h at room temperature, 1 mL of AcOH was added and the reaction mixture was concentrated. The residue was dissolved in 100 mL of 20:1 hexanes/EtOAc and the solution was filtered through a pad of silica gel. The filtrate was concentrated to give 11 g of the tite compound as a yellow oil.

1. stirringAfter stirring for 1 h at room temperature
2. concentrationthe reaction mixture was concentrated
3. dissolutionThe residue was dissolved in 100 mL of 20:1 hexanes/EtOAc
4. filtrationthe solution was filtered through a pad of silica gel
5. concentrationThe filtrate was concentrated