反应详情

温度

-78 °C

To a solution of 2,4-dibromothiazole (100 mg, 0.412 mmol) in 2 mL THF was added BuLi (1.6 M in THF, 283 μL, 0.453 mmol). The mixture was stirred at −78° C. for 15 min, then a solution of Intermediate 7.3 (134 mg, 0.412 mmol) in 0.6 mL THF was added dropwise. The mixture was stirred at −78° C. for 30 min, was allowed to warm to rt, then was quenched with sat. NH4Cl. The mixture was diluted with EtOAc, washed with H2O and brine, dried (Na2SO4) and concentrated. The crude product was purified by flash chromatography (0 to 40% EtOAc/hexanes gradient) followed by preparative HPLC purification to afford 39 mg of Intermediate 16.1.

1. stirringThe mixture was stirred at −78° C. for 30 min
2. temperatureto warm to rt
3. customwas quenched with sat. NH4Cl
4. additionThe mixture was diluted with EtOAc
5. washwashed with H2O and brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customThe crude product was purified by flash chromatography (0 to 40% EtOAc/hexanes gradient)
9. customfollowed by preparative HPLC purification