反应详情

To a 0° C. solution of 0.10 g of the product of Example 3 (0.30 mmols) in DMF (1.0 mL) was added 0.041 mL of triethylamine (0.30 mmols) and 0.056 g of 4-methoxybenzoylchloride (0.33 mmols). The reaction mixture was allowed to warm to rt and stirred for 23 h. The reaction mixture was diluted with 1 mL of water and 5 mL of EtOAc. The layers were separated, and the aqueous layer was extracted with EtOAc. The combined organics were washed with water and concentrated to a partial volume. Methanol was added, and a solid precipitated from the solution. The precipitate was filtered off and dried and the crude product was purified by silica gel chromatography to provide the title compound as a white powder (0.029 g, 21%). MS (ES+) m/e 473 [M+H]+.

1. customThe layers were separated
2. extractionthe aqueous layer was extracted with EtOAc
3. washThe combined organics were washed with water
4. concentrationconcentrated to a partial volume
5. additionMethanol was added
6. customa solid precipitated from the solution
7. filtrationThe precipitate was filtered off
8. customdried
9. customthe crude product was purified by silica gel chromatography