反应详情

温度

120 °C

In a glass tube was added successively 0.29 mmol 2-Iodo-5-methanesulfonyl-benzoic acid methyl ester (example B19(c)), 0.35 mmol 4-methylpyrazole, 0.59 mmol potassium carbonate, 0.06 mmol CuI and a solution of 0.12 mmol trans-1,2-diaminocyclohexane in 0.4 ml dioxane (degassed). The tube was filled with argon and sealed with a cap. The reaction mixture was heated at 120° C. overnight. The reaction mixture was cooled down to room temperature, dichloromethane and water were added. The aqueous phase was extracted 2 times with dichloromethane. The combined organic phases were dried over sodium sulfate and evaporated. The crude compound was purified on a log Flashpack cartridge. Eluent: Heptane/ethylacetate to provide the title compound (57%) as a light yellow oil. MS (m/e): 295.0([M+H]+, 100%).

1. additionThe tube was filled with argon
2. customsealed with a cap
3. temperatureThe reaction mixture was cooled down to room temperature
4. extractionThe aqueous phase was extracted 2 times with dichloromethane
5. dry with materialThe combined organic phases were dried over sodium sulfate
6. customevaporated
7. customThe crude compound was purified on a log Flashpack cartridge