反应详情

A mixture of 4-iodo-1-trityl-1H-imidazole (17.1 g, 39.2 mmol) and 4-bromomethyl-3-fluorobenzonitrile (9.65 g, 45.08 mmol) in 150 mL of dry acetonitrile is stirred at room temperature for 7 days. After concentration, the residue is mixed with methanol, and heated to reflux for 1.5 h. The solvent is subsequently removed and the residue is treated with 1M HCl (300 mL). The resulting suspension is filtered and the washed with HCl (1 M). The combined solution is adjusted to PH 9-10 by saturated NaHCO3 solution. The resulting precipitation is collected by filtration, dried in vacuum oven. MS (ESI) m/z (M+H) 328.1.

1. concentrationAfter concentration
2. additionthe residue is mixed with methanol
3. temperatureheated
4. temperatureto reflux for 1.5 h
5. customThe solvent is subsequently removed
6. additionthe residue is treated with 1M HCl (300 mL)
7. filtrationThe resulting suspension is filtered
8. washthe washed with HCl (1 M)
9. customThe resulting precipitation
10. filtrationis collected by filtration
11. customdried in vacuum oven