反应详情

The more polar diastereoisomer of (4-aminomethyl-1-phenyl-cyclohexyl)-dimethylamine (162.7 mg, 0.7 mmole) was added to a solution of [2-(1H-indol-3-yl)-1-methyl-ethyl]-carbamic acid phenyl ester (206 mg, 0.7 mmole) in dioxane (7 ml). The batch was then refluxed for 14 h. A precipitate formed at RT. The precipitate was filtered out, and washed once with cold dioxane (2 ml) and with diethyl ether (3×3 ml). The more polar diastereoisomer of 1-(4-dimethylamino-4-phenyl-cyclohexylmethyl)-3-[2-(1H-indol-3-yl)-1-methyl-ethyl]-urea was obtained in this manner as a colorless solid with a melting point of 140-146° C. in a yield of 231 mg (76%).

1. temperatureThe batch was then refluxed for 14 h
2. customA precipitate formed at RT
3. filtrationThe precipitate was filtered out
4. washwashed once with cold dioxane (2 ml) and with diethyl ether (3×3 ml)