反应详情

4-Bromo-2-methylphenol (10 g, 53.5 mmol) and 1-(2-chloroethyl)pyrrolidine HCl (11 g, 64.7 mmol) were heated at 80° C. in 500 mL of DMF in the presence of K2CO3 (22 g, 159.2 mmol) for 16 h. After cooling, the crude product was filtered and concentrated in vacuo. The brown oily residue was purified by PrepLC (SiO2; gradient of 90:8:2 to 85:10:5 hexanes-THF-TEA) to afford 11.25 g (39.6 mmol; 74%) of the title compound as a clear, colorless oil.

1. temperatureAfter cooling
2. filtrationthe crude product was filtered
3. concentrationconcentrated in vacuo
4. customThe brown oily residue was purified by PrepLC (SiO2; gradient of 90:8:2 to 85:10:5 hexanes-THF-TEA)