反应详情

温度

60 °C

To a sol. of compound 4 (39.2 g, 181 mmol) in dry toluene (500 mL) was added imidazole (61.5 g, 903 mmol), PPh3 (90 g, 343 mmol), and iodine (87.1 g, 343 mmol). This mixture was stirred at 60° C. for 2 h. The mixture was filtered over Celite, and the filtrate was concentrated under reduced pressure. Purification of the residue by FC (EtOAc/heptane 1:5→1:4→1:3→1:2→1:1) yielded the title compound (39.9 g, 67%).

1. filtrationThe mixture was filtered over Celite
2. concentrationthe filtrate was concentrated under reduced pressure
3. customPurification of the residue by FC (EtOAc/heptane 1:5→1:4→1:3→1:2→1:1)