反应详情

温度

100 °C

The compound of Example 1C (15 g, 24.2 mmol) and the compound of Example 1H (11 g, 26.5 mmol), were combined with NaI (2.7 g), and diisopropylethylamine (3.12 g) in 400 mL of acetonitrile in a 1 liter pressure bottle. The solution was heated at 100° C. TLC (EtOAc:hexane, 60:40) or HPLC was checked for the completion of the reaction; no starting material was observed after 16 hours. The reaction mixture was cooled to ambient temperature and filtered through Celite; the solvents were removed in vacuo. The crude material was diluted with EtOAc (500 mL) and washed with saturated ammonium chloride solution (2×100 ml). The solvent was removed in vacuo, and the crude material was loaded on silica gel column to elute with hexane/EtOAc (3:2-1:1-2:3). Pure fractions were collected and concentrated to provide 14.5 g (63.3%) of the titled compound.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. filtrationfiltered through Celite
3. customthe solvents were removed in vacuo
4. additionThe crude material was diluted with EtOAc (500 mL)
5. washwashed with saturated ammonium chloride solution (2×100 ml)
6. customThe solvent was removed in vacuo
7. washto elute with hexane/EtOAc (3:2-1:1-2:3)
8. customPure fractions were collected
9. concentrationconcentrated