反应详情

A mixture of (2R,6S,13aS,14aR,16aS,Z)-ethyl 6-amino-2-(3-fluorophenanthridin-6-yloxy)-5,16-dioxo-1,2,3,5,6,7,8,9,10,11,13a,14,14a,15,16,16a-hexadecahydrocyclopropa[e]pyrrolo[1,2-a][1,4]diazacyclopentadecine-14a-carboxylate (Example 1d, 1.11 g, 1.89 mmol) was dissolved in dimethylformamide (19 mL) and treated with N-methylmorpholine (0.73 ml, 6.6 mmol) followed by 5-methylisoxazole-3-carboxylic acid (0.264 g, 2.074 mmol) and HATU (0.860 g, 2.263 mmol). The reaction mixture was stirred at room temperature for 1 h, diluted with 2 N HCl and extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered, and evaporated under reduced pressure. The residue was purified by flash chromatography on silica gel, eluting with acetone/hexane, to provide the title compound (0.94 g, 72% yield).

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. customevaporated under reduced pressure
6. customThe residue was purified by flash chromatography on silica gel
7. washeluting with acetone/hexane