HRID353456
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
- 65 °C
PROCEDURE
实验过程
A solution of 1-(3-methoxyphenyl)piperazine dihydrobromide (3.5 g, 10 mmol) is dissolved in DMSO (30 mL) and heated at 65° C. for 4 h in a flask which is open to the atmosphere. After cooling, the mixture is poured into a separatory funnel containing 100 mL of 1 N sodium hydroxide solution and extracted with ethyl ether (3×100 mL). The organic extracts are dried (Na2SO4), filtered, and concentrated to provide 1-(4-bromo-3-methoxyphenyl)piperazine as a solid. 1H NMR (400 MHz, CDCl3) 7.34-7.36 (d, J=2.2 Hz, 1H,), 6.47 (s, 1H), 6.38-6.41 (d, J=2.8 Hz, 1H), 3.87 (s, 3H, OMe), 3.11-3.13 (m, 4H), 3.01-3.03 (m, 4H).
WORKUP
后处理
- temperatureAfter cooling
- additionthe mixture is poured into a separatory funnel
- extractionextracted with ethyl ether (3×100 mL)
- dry with materialThe organic extracts are dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated