反应详情

Compound 81b (95.0 mg, 0.23 0 mmol) and 2-bromothiazole (430 mg, 2.00 mmol) were placed in a vial and purged with Argon. Anhydrous DMF (2 mL) and DIEA (0.410 mL, 2.35 mmol) were added. The mixture was degassed and purged with Argon. CuI (2.24 mg, 0.0120 mmol) and dichloro(1,1′-bis(diphenylphosphino)ferrocene)palladium(II) dichloromethane adduct (16.5 mg, 0.0230 mmol) were added. The reaction was stirred at rt for 4 h. The reaction was filtered through a pad of diatomaceous earth and the filter cake was rinsed with EtOAc. The combined filtrates were washed with brine and water, dried, and concentrated. The residue was purified with preparative TLC (EtOAc/dichloromethane; 3:7) to obtain compound 81c. Mass Spectrum (LCMS, ESI pos.): Calcd. for C30H28N5O3S: 538.2 (M+H). found: 538.5.

1. custompurged with Argon
2. customThe mixture was degassed
3. custompurged with Argon
4. filtrationThe reaction was filtered through a pad of diatomaceous earth
5. washthe filter cake was rinsed with EtOAc
6. washThe combined filtrates were washed with brine and water
7. customdried
8. concentrationconcentrated
9. customThe residue was purified with preparative TLC (EtOAc/dichloromethane; 3:7)