反应详情

温度

85 °C

To a screw cap seal tube is added 0.83 g (2.0 mmol) of the product from Example 2, 0.25 g (0.82 mmol) of tri-o-tolylphosphine, 0.30 g (2.3 mmol) of N,N-diethyl acrylamide, 0.045 g (0.21 mmol) of palladium acetate, 40 mL of acetonitrile and 4 mL of triethylamine. The solution was purged with nitrogen then capped and heated to 85° C. for 15 hours. At the end of this time, the solution was concentrated, then taken up in 100 mL of water:ethyl acetate (1:2). The organic layer was separated and the water layer extracted once with ethyl acetate. The ethyl acetate layers were combined, dried (MgSO4) and concentrated. The residue subjected to column chromatography on silica. Elution first with 60% ethyl acetate:hexane followed by ethyl acetate:hexane:isopropanol (60:35:5) yielded 0.52 g of product (55%) which was crystallized from chloroform:acetone:hexane mp 159°-163° C. (soft).

1. customTo a screw cap
2. customseal tube
3. customThe solution was purged with nitrogen
4. customthen capped
5. concentrationAt the end of this time, the solution was concentrated
6. customThe organic layer was separated
7. extractionthe water layer extracted once with ethyl acetate
8. dry with materialdried (MgSO4)
9. concentrationconcentrated
10. washElution first with 60% ethyl acetate