HRID329396

反应详情

EQUATION

反应方程式

HRID 329396 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a 35 ml round-bottomed flask equipped with condenser and N2 inlet were added 0.75 g (2.59 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-aminothiazole hydrobromide, 0.69 g (2.59 mmol) of N-(3-trifluoromethylphenyl)piperazine hydrochloride, 1.08 ml (7.78 mmol) of triethylamine, 0.27 g (2.59 mmol) of sodium carbonate, 5 mg of sodium iodide, and 9.5 ml of ethanol. The reaction was heated at reflux, cooled, and taken up in ethyl acetate/water. The layers were separated, the ethyl acetate washed with brine, dried, and evaporated to give an oil. The oil was chromatographed on silica gel using ethyl acetate as eluent to give an oil. The oil was taken up in ethyl acetate/methanol, ether saturated with HCl was added, the precipitate filtered, washed with ether, and dried to give a white solid, 0.72 g (50%), m.p. 110°-115° 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
  4. temperaturecooled
  5. customThe layers were separated
  6. washthe ethyl acetate washed with brine
  7. customdried
  8. customevaporated
  9. customto give an oil
  10. customThe oil was chromatographed on silica gel
  11. customto give an oil
  12. filtrationthe precipitate filtered
  13. washwashed with ether
  14. customdried
  15. customto give a white solid, 0.72 g (50%), m.p. 110°-115° C.