反应详情

温度

140 °C

Lit. J. Am. Chem. Soc. 2001, 123, 7727-7729. To a stirred suspension of 0.58 mmol 5-iodo-1,3-dihydro-isoindole-2-carboxylic acid tert-butyl ester (Example A38(b)) in 4 ml dioxane were added 0.12 mmol copper(I) iodide, 1.74 mmol potassium carbonate, 0.17 mmol trans-1,2-diaminocyclohexane and 2.90 mmol 2-pyrrolidone and the reaction mixture was stirred at 140° C. for 16 h. The mixture was then cooled to room temperature, filtered, and the filtrate was concentrated in vacuo. The residue was purified by chromatography (SiO2, heptane/ethyl acetate) to yield the title compound as a white solid. MS (m/e): 247.3 ([M+H-Me2C═CH2]+, 100%).

1. temperatureThe mixture was then cooled to room temperature
2. filtrationfiltered
3. concentrationthe filtrate was concentrated in vacuo
4. customThe residue was purified by chromatography (SiO2, heptane/ethyl acetate)