反应详情

To polymer-supported triphenylphosphine (9.2 g; ˜27.5 mmol) in dichloromethane (40 mL) was added iodine (6.98 g; 27.5 mmol). The mixture was stirred for 30 minutes and then imidazole (1.87 g; 27.5 mmol) was added to the mixture. After stirring for 15 minutes a solution of 5-bromo-2-[2-(3-methoxy-2-methylphenyl)-ethyl]-phenylmethanol 8 (4.19 g; 12.5 mmol) in dichloromethane (100 mL) was added. The mixture was heated at reflux for 2 hours, cooled to room temperature and filtered. The filtrate was washed sequentially with sodium thiosulfate solution, water, and brine, dried over MgSO4, and concentrated to dryness at ambient temperature under high vacuum to give compound 9 as a yellow oil, 5.56 g.

1. additionwas added
2. temperatureThe mixture was heated
3. temperatureat reflux for 2 hours
4. filtrationfiltered
5. washThe filtrate was washed sequentially with sodium thiosulfate solution, water, and brine
6. dry with materialdried over MgSO4
7. concentrationconcentrated to dryness at ambient temperature under high vacuum