反应详情

温度

50 °C

Compound 3-4 (2.45 g; 8.32 mmol), methyl iodide (1.573 mL; 25.2 mmol), silver carbonate (3.28 g; 11.89 mmol) and chloroform (100 mL) were added to a sealed vessel. The contents of the sealed vessel were heated at 50° C. for 3 hours in the absence of light. The reaction was cooled to room temperature, the insoluble material filtered off, and the filtrate concentrated in vacuo. The crude material was purified via silica gel chromatography (0-10% EtOAc in hexane) to give the title compound. MS M+1=308.9. 1H NMR (CDCl3): 2.42 (s, 3H), 4.05 (s, 3H), 6.36 (s, 1), 7.16 (m, 1H), 7.24 (m, 1H), 7.44 (m, 1H).

1. temperatureThe reaction was cooled to room temperature
2. filtrationthe insoluble material filtered off
3. concentrationthe filtrate concentrated in vacuo
4. customThe crude material was purified via silica gel chromatography (0-10% EtOAc in hexane)