HRID736396
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
The product from Example 42C (56.1 mg, 0.250 mmol), triethylamine (55 μL, 0.39 mmol), 4-tert-butylaniline (52 μL, 0.33 mmol), and Pd(dppf)Cl2:CH2Cl2 (20.4 mg, 0.025 mmol) were combined in tetrahydrofuran (10 mL) and heated at 120° C. under a carbon monoxide atmosphere (700 psi) for 16 hours. The mixture was allowed to cool to room temperature and concentrated under reduced pressure. The residue was purified by flash chromatography (20% ethyl acetate in hexanes) to provide the title compound as a solid. 1H NMR (300 MHz, CDCl3) δ 8.51 (d, 1H), 7.96 (s, 4H), 7.82 (br s, 1H), 7.57 (d, 2H), 7.41 (d, 2H), 6.73 (d, 1H), 1.33 (s, 9H); MS (m/z) 321.
WORKUP
后处理
- temperatureto cool to room temperature
- concentrationconcentrated under reduced pressure
- customThe residue was purified by flash chromatography (20% ethyl acetate in hexanes)