HRID329037

反应详情

EQUATION

反应方程式

HRID 329037 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

17.6 g (0.117 mole) of sodium iodide were added to a solution of 40 g (0.17 mole) of 10-(3-chloropropyl)-2-trifluoromethyl-phenothiazine in 350 ml of methyl ethyl ketone followed by the addition of first 11.8 g (0.117 mole) of triethylamine and then 17 g (0.117 mole) of 2-(4-piperidyloxy)-ethanol. The resulting solution was refluxed for 20 hours and after cooling, the precipitate was removed by vacuum filtration. The filtrate was evaporated to dryness. The oil residue was stirred with a mixture of ether and dilute hydrochloric acid and the precipitate formed was recovered by vacuum filtration and crystallized from a 95% ethanol-ether mixture to obtain 40.5 g (71% yield) of 10-[3-(4-β-hydroxyethoxypiperidino) propyl]-2-trifluoromethyl-phenothiazine hydrochloride in the form of white crystals melting at 218°-219° C on a heated microscopic stage.

WORKUP

后处理

  1. temperatureThe resulting solution was refluxed for 20 hours
  2. temperatureafter cooling
  3. customthe precipitate was removed by vacuum filtration
  4. customThe filtrate was evaporated to dryness
  5. customthe precipitate formed
  6. filtrationwas recovered by vacuum filtration
  7. customcrystallized from a 95% ethanol-ether mixture