反应详情

To a 0° C. solution of 0.326 g of phenol, 1.8 ml of Hunig's base, and 2.5 ml of methylene chloride is added, via syringe, 1.07 g of product from Example 22 in 0.50 ml of methylene chloride. The reaction is stirred in an ice bath for 50 minutes; during which time the progress of reaction is checked by thin layer chromatography. The mixture is concentrated in vacuo, dissolved in ethyl acetate and washed with sodium bicarbonate. The organic layer is dried, concentrated in vacuo, and purified by chromatography (Silica Gel: ethyl acetate/hexane) to give 0.532 g of the desired product.

1. customduring which time the progress of reaction
2. concentrationThe mixture is concentrated in vacuo
3. dissolutiondissolved in ethyl acetate
4. washwashed with sodium bicarbonate
5. customThe organic layer is dried
6. concentrationconcentrated in vacuo
7. custompurified by chromatography (Silica Gel: ethyl acetate/hexane)