反应详情

温度

95 °C

A mixture of Example A1 (1 g, 3.97 mmol) in dioxane (20 mL) was sparged with Ar, treated with N,N-dimethyl urea (0.700 g, 7.95 mmol) and Cs2CO3 (1.942 g, 5.96 mmol), sparged with Ar, treated with dppf [1,1′-bis(diphenylphosphino)ferrocene] (12.38 g, 22.33 mmol) and Pd2(dba)3 (0.182 g, 0.199 mmol), sparged once again with Ar and heated at 95° C. overnight. The mixture was cooled to RT, treated with EtOAc and the solids removed via filtration through silica gel. The filtrate was concentrated to dryness and purified twice via silica gel chromatography (MeOH/DCM) to afford 1,1-dimethyl-3-(4-((6-nitropyridin-3-yl)oxy)pyridin-2-yl)urea (616 mg, 51%). MS (ESI) m/z: 304.1 (M+H+).

1. customsparged with Ar
2. customsparged once again with Ar
3. temperatureThe mixture was cooled to RT
4. additiontreated with EtOAc
5. customthe solids removed via filtration through silica gel
6. concentrationThe filtrate was concentrated to dryness
7. custompurified twice via silica gel chromatography (MeOH/DCM)