反应详情

温度

90 °C

A mixture of Example 126A (0.52 g, 1.25 mmol), 2-propyl-1,3,2-benzodioxaborole (0.50 g, 3.0 mmol), Pd(dppf)Cl2 (24 mg, 0.03 mmol) and Tl2CO3 (0.75 g, 1.6 mmol) in THF (15 mL) in a scintillation vial was purged with argon, sealed, and shaken at 90° C. for 72 hours. The mixture was treated with brine (25 mL) and extracted with ethyl acetate. The extract was dried (Mg2SO4), filtered, and concentrated. The residue was purified by flash column chromatography on silica gel eluting with 5% ethyl acetate/hexanes to provide the desired product (0.38 g, 80.0%). 1H NMR (CDCl3) δ 0.94 (t, 3H), 1.48 (s, 9H), 1.55 (m, 2H), 2.24 (s, 3H), 2.54 (t, 2H), 5.38 (s, 2H), 7.15 (d, 1H), 7.36-7.46 (m, 5H), 7.77 (d, 1H).

1. customsealed
2. extractionextracted with ethyl acetate
3. dry with materialThe extract was dried (Mg2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by flash column chromatography on silica gel eluting with 5% ethyl acetate/hexanes