反应详情

To a mixture of 2.61 g (0.04 mole) of zinc dust and 60 mL of DME was added 7.5 g (0.048 mole) of TiCl3. The reaction mixture was held at reflux for 2 h. A solutiom of 2.98 g (0.01 mole) of 11 was added dropwise in 1 h. The reaction mixture was held at reflux for 18 h, cooled and poured into water. The organic was extracted into ether. The ether layer was washed with brine and filtered through Celite. The filtrate was dried over MgSO4 and concentrated. The residual oil (2.5 g) was purified by HPLC to give 2.06 g (77%) of 12 as an oil in the second fraction.

1. temperatureat reflux for 2 h
2. temperatureat reflux for 18 h
3. temperaturecooled
4. extractionThe organic was extracted into ether
5. washThe ether layer was washed with brine
6. filtrationfiltered through Celite
7. dry with materialThe filtrate was dried over MgSO4
8. concentrationconcentrated
9. customThe residual oil (2.5 g) was purified by HPLC