反应详情

To a solution of the product of step 2 (0.7 g) and anhydrous triethylamine (0.7 ml) in dichloromethane (20 ml), 3-pyridin-3-ylacryloyl chloride hydrochloride (1.2 g) was added in batches in an ice-bath with the temperature no more than 5° C. After addition, the reaction was carried out for 30 min in an ice-bath, and then at room temperature overnight. The completion of reaction was indicated by TLC. Then potassium carbonate solution (10%) was added. The mixture was extracted with EtOAc (20 ml*3). The organic layer was dried over anhydrous MgSO4, filtered, and concentrated under reduced pressure to recover solvent. The residue was purified on silica gel column using EtOAc/petroleum ether/ethanol (2:1:5) as an eluent. The concentration of the eluent and crystallization provided a yellow solid powder.

1. additionAfter addition
2. customat room temperature
3. customovernight
4. customThe completion of reaction
5. extractionThe mixture was extracted with EtOAc (20 ml*3)
6. dry with materialThe organic layer was dried over anhydrous MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customto recover solvent
10. customThe residue was purified on silica gel column
11. customThe concentration of the eluent and crystallization
12. customprovided a yellow solid powder