反应详情

A solution of 1,6-heptadiyne (1.242 ml, 10.85 mmol) and ethyl cyanoformate (1.063 ml, 10.85 mmol) in dry degassed 1,4-dioxane (100 ml) under argon at rt was treated with cyclopentadienyl-Cobalt(I)-dicarbonyl (0.293 g, 1.628 mmol) and then heated at reflux for 18 h. Reaction was then evaporated, treated with toluene (100 ml), re-evaporated, dissolved in DCM (100 ml), filtered through a short pad of Kieselguhr, eluting with DCM, organic extracts evaporated, chromatographed (0-100% DCM:40-60 Petroleum ether then 0-10% methanol/DCM) to give product as an impure brown oil (427 mg, 21%).

1. customdegassed 1,4-dioxane (100 ml) under argon at rt
2. temperatureheated
3. temperatureat reflux for 18 h
4. customReaction
5. customwas then evaporated
6. additiontreated with toluene (100 ml)
7. customre-evaporated
8. dissolutiondissolved in DCM (100 ml)
9. filtrationfiltered through a short pad of Kieselguhr
10. washeluting with DCM, organic extracts
11. customevaporated
12. customchromatographed (0-100% DCM