反应详情

Step AAH (3): To a soln of 2,2-dimethyl-1,3-dioxane-4,6-dione (329 mg, 2.281 mmol) in dichloromethane (10 mL) was added DMAP (405 mg, 3.32 mmol). After stirring for 10 min, a solution of 4-(2-phenyl-1,3-dioxolan-2-yl)butanoyl chloride (2.07 mmol) in dichloromethane was added at 0° C. under nitrogen. The mixture was stirred at rt for 3 his. The crude reaction mixture was concentrated in vacuo. The residue was dissolved in EtOAc. The organic layer was sequentially washed with 1.0 N aqueous HCl, 1.0 N aqueous NaOH, and water. The organic layer was dried over Na2SO4, filtered and concentrated in vacuo to 2,2-dimethyl-5-(4-(2-phenyl-1,3-dioxolan-2-yl)butanoyl)-1,3-dioxane-4,6-dione (700 mg, 1.93 mmol, 93% yield).

1. stirringThe mixture was stirred at rt for 3 his
2. customThe crude reaction mixture
3. concentrationwas concentrated in vacuo
4. dissolutionThe residue was dissolved in EtOAc
5. washThe organic layer was sequentially washed with 1.0 N aqueous HCl, 1.0 N aqueous NaOH, and water
6. dry with materialThe organic layer was dried over Na2SO4
7. filtrationfiltered