反应详情

温度

125 °C

To a solution of 730 mg of the bromide prepared in Example 178a in 17.5 ml tetrahydrofuran were added 0.23 ml of methanol, 145 mg of trans-bis(acetato)-bis[o-(di-o-tolylphosphino)-benzyl]dipalladium(II), 877 mg of DBU and 760 mg of molybdenum hexacarbonyl This reaction mixture was then heated in the microwave (120 watts) for 20 minutes at 125° C. Seven further preparations were performed in the same manner and all worked up together. For this, they were concentrated in vacuo and the residue taken up in water and ethyl acetate. After phase separation, the aqueous phase was extracted three times with 75 ml portions of ethyl acetate and the combined organic phases washed with saturated sodium chloride solution, dried over sodium sulphate and concentrated in vacuo after filtration. The residue thus obtained was purified by twofold column chromatography on silica gel with hexane/0-30% ethyl acetate. Yield: 4.0 g of the title compound.

1. concentrationFor this, they were concentrated in vacuo
2. customAfter phase separation
3. extractionthe aqueous phase was extracted three times with 75 ml portions of ethyl acetate
4. washthe combined organic phases washed with saturated sodium chloride solution
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated in vacuo
7. filtrationafter filtration
8. customThe residue thus obtained
9. customwas purified by twofold column chromatography on silica gel with hexane/0-30% ethyl acetate