反应详情

A solution of the product from Example 100 (0.1 g, 0.324 mmol) in tetrahydrofuran (4 ml) at −78° C. was treated with a i 0.6M solution of n-butyllithium (0.6 ml, 0.97 mmol) in hexanes. After 5 minutes the mixture was treated with dimethylformamide (0.3 ml) and allowed to reach room temperature. After 30 minutes at room temperature the reaction was carefully quenched with water and extracted into dichloromethane (×2). The organic layer was then washed with brine, dried (Na2SO4) and reduced in vacuo. The residue was purified by silica gel chromatography eluting with ethyl acetate, to afford the title compound, (0.0349, 41%); MS (ES+) m/e 259 [M+H]+.

1. customto reach room temperature
2. customAfter 30 minutes at room temperature the reaction was carefully quenched with water
3. extractionextracted into dichloromethane (×2)
4. washThe organic layer was then washed with brine
5. dry with materialdried (Na2SO4)
6. customThe residue was purified by silica gel chromatography
7. washeluting with ethyl acetate