反应详情

A cooled (−78° C.) solution of 1-2 (2 g, 9.84 mmol) in Et2O (50 ml) was treated with LDA (9.84 ml, 19.68 mmol) and stirred for 1 h. The mixture was treated with dimethyl carbonate (1.658 ml, 19.68 mmol), warmed to RT and stirred overnight. The mixture was quenched with 1N HCl and extracted twice with EtOAc. The organic phase was dried over Na2SO4, filtered and concentrated. The crude material was purified by gradient elution on silica gel (0 to 60% EtOAc in Hex) to yield a 1:1 mixture of 1-3 and starting material as a tan oil. Data for 1-3: LRMS m/z (M+H): 262.1.

1. stirringstirred overnight
2. customThe mixture was quenched with 1N HCl
3. extractionextracted twice with EtOAc
4. dry with materialThe organic phase was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude material was purified by gradient elution on silica gel (0 to 60% EtOAc in Hex)
8. customto yield
9. additiona 1:1 mixture of 1-3