反应详情

温度

100 °C

The product from Example 33A (0.1520 g, 0.396 mmoles), methyl-4-bromobenzoate (0.1702 g, 0.792 mmoles), K3PO4 (0.1680 g, 0.792 mmoles), Pd(OAc)2 (0.0070 g, 0.032 mmoles), and 2-(di-tert-butylphosphino)biphenyl (0.0140 g, 0.048 mmoles) was treated with toluene (1.16 mL) under a nitrogen atmosphere. The resulting red solution was degassed, stirred for 10 min, and heated to 100° C. overnight. The black solution was diluted with diethyl ether, extracted with sat. NH4Cl and sat. NaCl, dried (Na2SO4), and concentrated under reduced pressure. The residue was purified by flash chromatography (10:1 hexane:ethyl acetate) on silica gel to provide the title compound (0.1886 g, 92%) as a yellow oil.

1. customThe resulting red solution was degassed
2. additionThe black solution was diluted with diethyl ether
3. extractionextracted with sat. NH4Cl and sat. NaCl
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by flash chromatography (10:1 hexane:ethyl acetate) on silica gel