反应详情

To (4-bromo-3-thienyl)(3-chlorophenyl)methanol from Example 3, Step 1 (144 mg, 0.474 mmol) in CH2Cl2 (1 mL) at 0° C., were successively added triethylsilane (303 μL, 1.90 mmol), quickly and TFA (364 μL, 4.74 mmol) dropwise. After 30 min., the reaction was concentrated to dryness and the residue was dissovled in CHCl3 and washed with 5% aq. NaHCO3. The aqueous layer was extracted with CHCl3 and the combined organics were washed with water and brine, dried (Na2SO4) and concentrated. The crude product was purified on silica gel (toluene/hexane 5:95) to afford the desired product as a colorless oil.

1. customat 0° C.
2. concentrationthe reaction was concentrated to dryness
3. washwashed with 5% aq. NaHCO3
4. extractionThe aqueous layer was extracted with CHCl3
5. washthe combined organics were washed with water and brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customThe crude product was purified on silica gel (toluene/hexane 5:95)