反应详情

To a mixture of 6-2 (8.64 g, 29.48 mmol) and 6-4 (5.0 g, 32.4 mmol) in Et3N (50 mL) at 0° was added CuI (0.14 g, 0.74). The solution was purged with argon and [(C6H5)3P]2PdCl2 (0.52 g, 0.74 mmol) was added. After 1 h the cooling bath was removed and the solution was stirred for an additional 12 h. The solution was diluted with diethyl ether (250 mL) and washed with water (4×100 ml) followed by brine (100 mL). The etheral layer was dried (Na2SO4), concentrated, and chromatographed (silica gel, 30% ethyl acetate/hexanes) to give 8.6 g of 6-5.

1. additionwas added
2. customAfter 1 h the cooling bath was removed
3. additionThe solution was diluted with diethyl ether (250 mL)
4. washwashed with water (4×100 ml)
5. dry with materialThe etheral layer was dried (Na2SO4)
6. concentrationconcentrated
7. customchromatographed (silica gel, 30% ethyl acetate/hexanes)