反应详情

温度

120 °C

Lit. Org. Lett. 2002, 4(20), 3517-3520. To a stirred suspension of 0.66 mmol 5-chloro-6-iodo-1,3-dihydro-isoindole-2-carboxylic acid tert-butyl ester (Example A3(c)) in 5 ml isopropanol were added 1.32 mmol ethylene glycol, 0.07 mmol copper(I) iodide, 1.32 mmol cesium carbonate, 0.13 mmol 1,20-phenanthroline and 3.29 mmol ethyl mercaptan and the reaction mixture was stirred at 120° C. for 1 h. The mixture was then cooled to room temperature and 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): 260.0 ({37Cl}[M+H-Me2C═CH2]+, 42%), 258.1 ({35Cl}[M+H-Me2C═CH2]+, 100%).

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