HRID394055
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
- 160 °C
PROCEDURE
实验过程
To a suspension of 340 mg of N-(2,6-dichlorophenyl)-3-(2,6-dibromo-4-methoxyphenyl)-propionamide in 20 mL of pyridine was added CuI (137 mg) and powdered, dried K2CO3 (99 mg). The resulting mixture was heated to 160° C. in a sealed tube overnight (20 h), then concentrated. The reside was purified by flash chromatography on a Biotage 40S column, eluting with 100% CH2Cl2, to yield 5-Bromo-1-(2,6-dichlorophenyl)-3,4-dihydro-7-methoxy-2(1H)-quinolinone as a white solid. Mass spectrum (ESI) 402.0 (M+1). 1H NMR (500 MHz, CDCl3): δ 7.48 (d, J=8.0 Hz, 2H); 7.34 (t, J=8.0 Hz, 1H); 6.83 (d, J=2.5 Hz, 1H); 5.77 (d, J=2.5 Hz, 1H); 3.67 (s, 3H); 3.18 (m, 2H); 2.84 (m, 2H).
WORKUP
后处理
- concentrationconcentrated
- customThe reside was purified by flash chromatography on a Biotage 40S column
- washeluting with 100% CH2Cl2