HRID329393

反应详情

EQUATION

反应方程式

HRID 329393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a 35 ml round-bottomed flask equipped with condenser and N2 inlet were added 3.19 g (10 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-aminothiazole hydrobromide, 2.12 g (10 mmol) of N-(1-naphthyl)piperazine, 2.79 ml (20 mmol) of triethylamine, 1.06 g (10 mmol) of sodium carbonate, 2 mg of sodium iodide, and 25 ml of ethanol. The reaction was heated at reflux for 5 days, cooled, and the precipitate filtered, and washed with ethanol and water. The orange solid was chromatographed on silica gel using ethyl acetate/methylene chloride as eluent to give a white solid. The solid was taken up in ethyl acetate/methanol, ether saturated with HCl added, the precipitate filtered, washed with ether, and dried to give a white solid, 1.61 g (31%), m.p. 274°-277° C.

WORKUP

后处理

  1. customTo a 35 ml round-bottomed flask equipped with condenser and N2 inlet
  2. temperatureThe reaction was heated
  3. temperatureat reflux for 5 days
  4. temperaturecooled
  5. filtrationthe precipitate filtered
  6. washwashed with ethanol and water
  7. customThe orange solid was chromatographed on silica gel
  8. customto give a white solid
  9. filtrationthe precipitate filtered
  10. washwashed with ether
  11. customdried
  12. customto give a white solid, 1.61 g (31%), m.p. 274°-277° C.