反应详情

温度

120 °C

A mixture of 2-chloro-N-(4-chlorophenyl)-N-isopropyl-1-methyl-1H-benzimidazol-7-amine (30 mg, 0.90 mmol) and 4-chloro-2-methoxy-6-methylaniline (46 mg, 0.27 mmol) was stirred at 120° C. for 19 h. The mixture was dissolved in ethyl acetate (30 ml), washed with saturated aqueous sodium bicarbonate (15 ml) and water (10 ml), dried over magnesium sulfate and evaporated in vacuo. The residue was purified by reverse phase HPLC (acetonitrile containing 0.1 trifluoroacetic acid/water containing 0.1% trifluoroacetic acid). The fraction was concentrated to dryness, dissolved in methanol (10 ml) and treated with 2 M hydrogen chloride in diethyl ether (2 ml) and evaporated in vacuo to give 7.8 mg (19%) of the title compound as a powder.

1. washwashed with saturated aqueous sodium bicarbonate (15 ml) and water (10 ml)
2. dry with materialdried over magnesium sulfate
3. customevaporated in vacuo
4. customThe residue was purified by reverse phase HPLC (acetonitrile containing 0.1 trifluoroacetic acid/water containing 0.1% trifluoroacetic acid)
5. concentrationThe fraction was concentrated to dryness
6. dissolutiondissolved in methanol (10 ml)
7. additiontreated with 2 M hydrogen chloride in diethyl ether (2 ml)
8. customevaporated in vacuo