反应详情

温度

23 °C

To a solution of 2-(4-iodo-imidazol-1-yl)-4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyridine (example E.23) (4.83 g, 10 mmol) in THF (50 mL) at 0° C. was quickly added added i-PrMgCl.LiCl (1 M in THF, 11 mL, 11 mmol) and the mixture was stirred at 0° C. for 15 min. Then Bu3SnCl (3.25 mL, 12 mmol) was added, the cooling bath was removed and the mixture was stirred at 23° C. for 14 h. Poured into sat. NH4Cl-sol., extracted with EtOAc, washed with brine and dried over Na2SO4. Removal of the solvent in vacuum left a brown oil, which was purified by quick silica gel column chromatography with heptane/EtOAc 4:1 gave a yellow oil (4.42 g, 62%, ca. 90% pure). MS (ISP) 647.3 [(M+H)+].

1. customthe cooling bath was removed
2. additionPoured into sat. NH4Cl-sol
3. extraction, extracted with EtOAc
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. customRemoval of the solvent in vacuum
7. waitleft a brown oil, which
8. customwas purified by quick silica gel column chromatography with heptane/EtOAc 4:1
9. customgave a yellow oil (4.42 g, 62%, ca. 90% pure)