反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
A mixture of 4-(5-bromopentyl)-1,1′-biphenyl (331 mg, 1.09 mmol) and 2,4-lutidine (1 mL) was heated at 60-70° C. for 12 hrs. The resulted mixture was washed with diethyl ether and then dissolved in water (15 mL). The aqueous solution was extracted with diethyl ether (30 mL×3). Water was removed by lyophilization to afford 342 mg of the title compound. Yield: 77%. 1H NMR (300 MHz, CDCl3) δ 1.51 (m, 2H), 1.71 (m, 2H), 1.92 (m, 2H), 2.55 (s, 3H), 2.65 (t, J=7.8 Hz, 2H), 2.84 (s, 3H), 4.73 (t, J=7.8 Hz, 2H), 7.20-7.75 (m, 11H), 9.31 (d, J=6.3 Hz, 1H) ppm; 13C NMR (75 MHz, CDCl3) δ 20.1, 22.0, 25.8, 30.5, 30.8, 35.2, 57.4, 126.7, 126.9, 127.0, 128.2, 128.6, 128.8, 130.4, 138.5, 140.7, 140.9, 145.4, 152.8, 158.4 ppm.
WORKUP
后处理
- washThe resulted mixture was washed with diethyl ether
- dissolutiondissolved in water (15 mL)
- extractionThe aqueous solution was extracted with diethyl ether (30 mL×3)
- customWater was removed by lyophilization