反应详情

温度

140 °C

N1,N1,N2-Trimethylethane-1,2-diamine (221 mg, 2.16 mmol) was added to a suspension of N-(4-Fluoro-2-methoxy-5-nitrophenyl)-5-methyl-4-(1-methylindol-3-yl)pyrimidin-2-amine (Intermediate 79, 400 mg, 0.98 mmol) in DMA (4 mL). The mixture was heated in a microwave at 140° C. for 0.5 h. The mixture was then concentrated in vacuo and the residue was dissolved in EtOAc (100 mL). This solution was washed with water (2×100 mL) and sat. brine (100 mL), dried (MgSO4) and concentrated in vacuo. Purification by FCC, eluting with 1-8% methanolic ammonia in CH2Cl2 gave the title compound (202 mg, 42%) as an orange dry film; m/z: ES+ MH+ 444.55.

1. concentrationThe mixture was then concentrated in vacuo
2. dissolutionthe residue was dissolved in EtOAc (100 mL)
3. washThis solution was washed with water (2×100 mL) and sat. brine (100 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customPurification by FCC
7. washeluting with 1-8% methanolic ammonia in CH2Cl2