反应详情

温度

100 °C

A mixture of Example A1 (6 g, 23.8 mmol) in dioxane (100 mL) was sparged with Ar under sonication for 20 min, then treated with N,N-dimethyl urea (10.50 g, 119 mmol), Cs2CO3 (1.942 g, 5.96 mmol), and XANTPHOS (2.76 g, 4.77 mmol), and again sparged with Ar under sonication for 15 min. Pd2(dba)3 (2.18 g, 2.38 mmol) was added and the mixture was again sparged with Ar for 15 min under sonication. The reaction was then heated to 100° C. for 3 h. The mixture was cooled to RT, diluted with EtOAc and the solids removed via filtration through diatomaceous earth. The filtrate was concentrated to dryness and purified by silica gel chromatography (MeOH/DCM) to afford 1,1-dimethyl-3-(4-((6-nitropyridin-3-yl)oxy)pyridin-2-yl)urea (6.22 g, 81%). MS (ESI) m/z: 304.1 (M+H+).

1. customagain sparged with Ar under sonication for 15 min
2. customthe mixture was again sparged with Ar for 15 min under sonication
3. temperatureThe mixture was cooled to RT
4. additiondiluted with EtOAc
5. customthe solids removed via filtration through diatomaceous earth
6. concentrationThe filtrate was concentrated to dryness
7. custompurified by silica gel chromatography (MeOH/DCM)