HRID329038

反应详情

EQUATION

反应方程式

HRID 329038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

22.5 g (0.15 mole) of sodium iodide were added to a solution of 51.5 g (0.15 mole) of 10-(3-chloropropyl)-2-trifluoromethyl-phenothiazine in 400 ml of methyl ethyl ketone followed by the addition of 15.2 g (0.15 mole) of triethylamine and then 26 g (0.15 mole) of 1,2-dimethyl-2-(4-piperidyloxy)-ethanol. The mixture was then refluxed for 20 hours and after cooling, the precipitate formed was removed by vacuum filtration. The filtrate was evaporated to dryness and the oil residue was chromatographed over 1 kg of neutral alumina. Elution with ethyl acetate gave 34.5 g (48% yield) of 2-trifluoromethyl-10-[3-(4-[1,2-dimethyl-2-hydroxyethoxy]-piperidino)-propyl]-phenothiazine in the form of a clear amber oil.

WORKUP

后处理

  1. temperatureThe mixture was then refluxed for 20 hours
  2. temperatureafter cooling
  3. customthe precipitate formed
  4. customwas removed by vacuum filtration
  5. customThe filtrate was evaporated to dryness
  6. customthe oil residue was chromatographed over 1 kg of neutral alumina
  7. washElution with ethyl acetate