反应详情

温度

85 °C

To a screw cap seal tube is added 0.84 g (2.0 mmol) of the product from Example 2, 0.20 g (0.66 mmol) of tri-o-tolylphosphine, 0.21 g (2.1 mmol) of N,N-dimethyl acrylamide, 0.040 g (0.2 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 3 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 an the residue subjected to column chromatography on silica. Elution with 50% ethyl acetate:hexane then ethyl acetate:hexane:isopropanol (60:35:5) yielded 0.63 g of product which was crystallized from chloroform:acetone:hexane to yield 0.47 g of product as a yellow solid, m.p. 208°-211° C.

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 an the residue
10. washElution with 50% ethyl acetate