反应详情

温度

-60 °C

To a stirred solution of Compound 80 (0.254 g, 1 mmol) in dry CH2 Cl2 (5 ml) was added a solution of TiCl4 in CH2Cl2 (1M, 3 ml) with cooling (-60° C.). After 3 min., to this was added dichloromethyl methyl ether (0.46 g, 4 mmol) dropwise. The reaction mixture was stirred at same temperature for 1 hr. The mixture was poured into water and stirred at room temperature for 15 min. The organic layer was separated and the aqueous layer was extracted with Et2O (50 ml×2). The combined solution was washed with brine, dried (MgSO4) and concentrated in vacuo to give crude product. The crude product was purified by a column chromatography to give Compound 81 (86 mg) as an oil

1. stirringstirred at room temperature for 15 min
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted with Et2O (50 ml×2)
4. washThe combined solution was washed with brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customto give crude product
8. customThe crude product was purified by a column chromatography