反应详情

To a suspension of NaH (909 mg/22.7 mmol) in THF (50 ml) was added 3-(tritylamino)-1-propanol, and the solution was stirred at reflux temperature for 2 hours. To the solution was added α,α′-dibromo-o-xylene, and the solution was stirred at reflux temperature for 16 hours. After cooling, the mixture was poured into water. The whole was extracted with ethyl acetate (100 ml×2). The combined organic layer was washed with brine (30 ml), dried over magnesium sulfate, filtered and concentrated. The residue was purified by column chromatography (SiO2, 200-350 mesh/hexane:ethyl acetate=100:0-20:1) to afford a yellow oil (4.84 g/51%).

1. temperatureat reflux temperature for 2 hours
2. stirringthe solution was stirred
3. temperatureat reflux temperature for 16 hours
4. temperatureAfter cooling
5. extractionThe whole was extracted with ethyl acetate (100 ml×2)
6. washThe combined organic layer was washed with brine (30 ml)
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated
10. customThe residue was purified by column chromatography (SiO2, 200-350 mesh/hexane:ethyl acetate=100:0-20:1)
11. customto afford a yellow oil (4.84 g/51%)