反应详情

Tetrakis(triphenylphosphine)-palladium (0) (1.48 g, 1.3 mmol) was added to a solution of (9) (13.8 g, 26 mmol) and (8) (22.6 g, 77 mmol) in a mixture of ethanol (100 mL), 2M aqueous sodium carbonate (100 mL) and toluene (300 mL) that had been deoxygenated with argon. The solution was deoxygenated and heated at reflux for 16 hours, then poured into methanol. The resulting brown precipitate was filtered, dissolved in chloroform, washed with brine, and dried over magnesium sulfate. The solution was poured into methanol, and the brown precipitate filtered to give (10) (22.4 g, 99%).

1. customhad been deoxygenated with argon
2. customThe solution was deoxygenated
3. temperatureheated
4. temperatureat reflux for 16 hours
5. additionpoured into methanol
6. filtrationThe resulting brown precipitate was filtered
7. dissolutiondissolved in chloroform
8. washwashed with brine
9. dry with materialdried over magnesium sulfate
10. additionThe solution was poured into methanol
11. filtrationthe brown precipitate filtered