反应详情

温度

80 °C

The compound of Example 10B (0.95 g, 3.9 mmol) was dissolved in 3 mL of dimethylformamide; 1 mL of 1-(trimethylsilyl)imidazole was added, and the resultant solution was stirred overnight at ambient temperature, then heated at 80° C. for 8 hours. The crude mixture was partitioned between ethyl acetate and water; the organic phase was washed with brine and dried over Na2SO4. The solvents were removed in vacuo, and the residue was purified by chromatography on an Analogix Intelliflash 280™, eluting with a gradient of 0% to 20% ethyl acetate in hexanes to provide the titled compound (1.18 g, 96%).

1. customThe crude mixture was partitioned between ethyl acetate and water
2. washthe organic phase was washed with brine
3. dry with materialdried over Na2SO4
4. customThe solvents were removed in vacuo
5. customthe residue was purified by chromatography on an Analogix Intelliflash 280™
6. washeluting with a gradient of 0% to 20% ethyl acetate in hexanes