反应详情

To a room temperature suspension of 0.036 g of nicotinic acid (0.30 mmols) and 0.061 g of EDCI (0.32 mmols) in dry DMF (2.0 mL) was added 0.043 g of HOBt (0.32 mmols). After stirring for 10 min., 0.10 g of the product of Example 3 (0.3 mmols) was added to the reaction mixture. After stirring for 1 h, the reaction was treated with an additional 0.061 g of EDCI (0.32 mmols). The mixture was allowed to stir for 27 h at rt. The reaction mixture was diluted with 2 mL of water and 10 mL of EtOAc. The layers were separated, and the organic layer was washed with water. The organics were dried over MgSO4, filtered, and concentrated. The yellow residue was washed with methanol to yield an off-white solid (73 mg, 57%). MS (ES+) m/e 444 [M+H]+.

1. stirringAfter stirring for 1 h
2. stirringto stir for 27 h at rt
3. customThe layers were separated
4. washthe organic layer was washed with water
5. dry with materialThe organics were dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. washThe yellow residue was washed with methanol