HRID387641

反应详情

EQUATION

反应方程式

HRID 387641 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.5 g of 2-(2-bromophenyl)ethyl methanesulfonate, 5.59 g of 2-ethoxyethanamine, 8.67 g of potassium carbonate and 70 cm3 of tetrahydrofuran are stirred under the reflux of the solvent under an inert atmosphere for 48 h. The heating is stopped, then the reaction mixture is filtered. The insoluble material is washed twice with ethyl acetate. The filtrate is concentrated using a rotary evaporator under reduced pressure (5 kPa). The product obtained is purified by flash chromatography over silica (column: 330 g; particle size: 20-40 μm, spherical; eluent: 100% ethyl acetate to 90% ethyl acetate/10% methanol gradient). After concentrating the fractions under reduced pressure, 2.45 g of 2-(2-bromophenyl)-N-(2-ethoxyethyl)ethanamine are obtained in the form of a yellow oil.

WORKUP

后处理

  1. temperaturereflux of the solvent under an inert atmosphere for 48 h
  2. filtrationthe reaction mixture is filtered
  3. washThe insoluble material is washed twice with ethyl acetate
  4. concentrationThe filtrate is concentrated
  5. customa rotary evaporator under reduced pressure (5 kPa)
  6. customThe product obtained
  7. customis purified by flash chromatography over silica (column: 330 g; particle size: 20-40 μm, spherical; eluent: 100% ethyl acetate to 90% ethyl acetate/10% methanol gradient)
  8. concentrationAfter concentrating the fractions under reduced pressure, 2.45 g of 2-(2-bromophenyl)-N-(2-ethoxyethyl)ethanamine
  9. customare obtained in the form of a yellow oil