HRID329404

反应详情

EQUATION

反应方程式

HRID 329404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 125 ml round-bottomed flask equipped with condenser and N2 inlet were added 2.39 g (7.5 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-methylthiazole hydrobromide, 2.0 g (7.5 mmol) of N-(3-trifluoromethylphenyl)piperazine hydrochloride, 2.62 ml (15.0 mmol) of diisopropylethylamine, 1.59 g (15.0 mmol) of sodium carbonate, 5 mg of sodium iodide, and 50 ml of methylisobutylketone. The reaction was heated at reflux for 4.5 days, filtered hot to remove inorganic material, cooled, and the precipitate filtered and washed with ether and ethyl acetate. The solid was taken up in methylene chloride, hydrochloride gas bubbled through to precipitate the salt, and the resulting solid filtered, washed with methylene chloride, and dried to give a solid, m.p. 170°-175° C., 1.93 g (51%).

WORKUP

后处理

  1. customTo a 125 ml round-bottomed flask equipped with condenser and N2 inlet
  2. temperatureThe reaction was heated
  3. temperatureat reflux for 4.5 days
  4. filtrationfiltered hot
  5. customto remove inorganic material
  6. temperaturecooled
  7. filtrationthe precipitate filtered
  8. washwashed with ether and ethyl acetate
  9. custombubbled through
  10. customto precipitate the salt
  11. filtrationthe resulting solid filtered
  12. washwashed with methylene chloride
  13. customdried
  14. customto give a solid, m.p. 170°-175° C., 1.93 g (51%)