反应详情

温度

100 °C

A suspension of 2-methylthio-4-[5-(2-chloro-pyrimidin-4-yl)benzimidazol-1-yl]pyrimidine (EXAMPLE 34; 85 mg), 2,4,6-trimethoxybenzylamine hydrochloride (160 mg), and diisopropylethylamine (210 mL) in 3 mL of DMSO was heated to 100° C., at which point all solids were dissolved. The mixture was stirred at 100° C. for 20 h, then cooled and diluted with 15 mL of 1:1 EtOAc-Et2O, washed with 2×5 mL of water and 5 mL of brine, dried over Na2SO4 and concentrated. The residue was purified by preparative thin-layer chromatography) eluting with 95:5 CH2Cl2—MeOH to provide 98 mg of the title compound. Mass spectrum (ESI) 516.4 (M+1).

1. dissolutionwere dissolved
2. temperaturecooled
3. washwashed with 2×5 mL of water and 5 mL of brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe residue was purified by preparative thin-layer chromatography)
7. washeluting with 95:5 CH2Cl2—MeOH