反应详情

To the stirred solution of starting material 7 (0.85 g, 3.66 mmol) in dry CH2Cl2 added Imidazole (0.5 g, 7.32 mmol) and TESCl (0.6 mL, 3.66 mmol) sequentially at 0° C. under argon atmosphere and stirred the reaction mixture at same temperature for 6 h. Then reaction mixture was diluted with H2O (10 mL) followed by extraction with CH2Cl2 (50 mL), brine (25 mL), dried (Na2SO4) and concentrated in vacuo. Purification by column chromatography (SiO2, 5 to 10% EtOAc in petroleum ether eluant) gave pure compound 8 (0.85 g, 88%) as syrup.

1. customThen reaction mixture
2. extractionfollowed by extraction with CH2Cl2 (50 mL), brine (25 mL)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated in vacuo
5. customPurification by column chromatography (SiO2, 5 to 10% EtOAc in petroleum ether eluant)