HRID1106862

反应详情

EQUATION

反应方程式

HRID 1106862 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

2-(3,4-Dimethoxyphenyl)-N-methylethylamine (2.77 ml, 0.015 mol) and 2-bromoethanol (1.13 ml, 0.015 mol) were dissolved in N,N-dimethylformamide (10 ml). To the resulting solution, potassium iodide (2.45 g, 0.015 mol) was added, followed by stirring at 80° C. for 1.5 h. The reaction mixture was cooled to room temperature and, thereafter the solvent was evaporated under vacuum; after adding a saturated aqueous solution of sodium bicarbonate, three extractions were conducted with ethyl acetate. The organic layers were combined, dried with sodium sulfate and concentrated under vacuum. The residue was purified by being subjected to column chromatography on silica gel using a 9:1 solvent system of chloroform and methanol as an eluent and the fractions containing the end product were collected and the solvent was evaporated under vacuum, followed by drying to yield the end compound 2-[N-(3,4-dimethoxyphenethyl)-N-methylamino]ethanol (1.35 g) as an oil.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customthe solvent was evaporated under vacuum
  3. additionafter adding
  4. extractiona saturated aqueous solution of sodium bicarbonate, three extractions
  5. dry with materialdried with sodium sulfate
  6. concentrationconcentrated under vacuum
  7. customThe residue was purified
  8. additionthe fractions containing the end product
  9. customwere collected
  10. customthe solvent was evaporated under vacuum
  11. customby drying