反应详情

A solution of alkyne 19 (5.547 g, 15.2 mmol) in dichloromethane (50 mL) was treated with Cp2ZrHCl (5.794 g, 22.5 mmol). The reaction was stirred for 45 min. and then N-iodosuccinimide (4.966 g, 22.1 mmol) was added. After 15 min., saturated sodium bicarbonate solution (200 mL) was added and the mixture was extracted with dichloromethane (2×100 mL). The combined dichloromethane solution was dried (MgSO4), filtered and evaporated. Purification by flash chromatography on silica gel (0-5% ethyl acetate/hexanes) gave 6.608 g (13.1 mmol, 86%) of the vinyl iodide (32).

1. waitAfter 15 min.
2. extractionthe mixture was extracted with dichloromethane (2×100 mL)
3. dry with materialThe combined dichloromethane solution was dried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customPurification by flash chromatography on silica gel (0-5% ethyl acetate/hexanes)