反应详情

温度

130 °C

A mixture of 2,4-dichloro-7-(1-ethylpropyl)-1-methyl-1H-benzimidazole (140 mg, 0.52 mmol), 4-bromo-2-methoxy-6-methylaniline (335 mg, 1.55 mmol) and 1-methyl-2-pyrrolidone (5 drops) was stirred at 130° C. for 2 days under nitrogen atmosphere. The mixture was dissolved in ethyl acetate/water, extracted with ethyl acetate and washed with brine. The organic layer was dried over magnesium sulfate, and concentrated to give a brown oil. The oil was subjected to chromatography on a silica gel (n-hexane/ethyl acetate=10:1-1:1) and crystallized from iso-propanol to afford the title compound as colorless crystals (115 mg, 49%). mp. 218-220° C.

1. extractionextracted with ethyl acetate
2. washwashed with brine
3. dry with materialThe organic layer was dried over magnesium sulfate
4. concentrationconcentrated
5. customto give a brown oil
6. customcrystallized from iso-propanol