反应详情

A solution of 2-(pyridine-2-ylamino)-thiazole-5-carbaldehyde (0.10 g, 0.49 mmol, WO2004/001059), benzene-1,4-diamine (0.105 g, 0.97 mmol) and triethylsilane (0.19 mL, 1.2 mmol) in CH2Cl2-TFA (3:1, 4 mL) was stirred at ambient temperature for 4 h. The reaction mixture was concentrated in vacuo and the residue partitioned between CH2Cl2 and saturated aqueous NaHCO3 solution. The organic phase was washed with saturated aqueous NaHCO3 solution, brine, dried (MgSO4) and concentrated in vacuo. The crude product which contained the title compound along with the starting aldehyde and benzene-1,4-diamine was carried on directly into the next step.

1. concentrationThe reaction mixture was concentrated in vacuo
2. customthe residue partitioned between CH2Cl2 and saturated aqueous NaHCO3 solution
3. washThe organic phase was washed with saturated aqueous NaHCO3 solution, brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo