HRID329049

反应详情

EQUATION

反应方程式

HRID 329049 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

14.1 g of 2-trifluoromethyl-10-(3-chloropropyl)-phenothiazine were dissolved in 50 ml of methyl ethyl ketone and 6.14 g of sodium iodide, 4.15 g of triethylamine, then 10 g of 2-(4-heptyl-4-piperidyloxy)-ethanol dissolved in 50 ml of methyl ethyl ketone were successively added thereto. The mixture was refluxed with agitation for 40 hours and after cooling, the precipitate formed was removed by vacuum filtration. The organic solution was washed with an aqueous solution of sodium bicarbonate, then with water, dried and then concentrated. The said product was reacted with an ether solution of hydrogen chloride and the obtained precipitate was recovered by vacuum filtration and was crystallized from an ethanol ether mixture to obtain 7.8 g of 2-trifluoromethyl-10-[3-(4-heptyl-4-β-hydroxy-ethoxy-piperidino)-β-propyl]-phenothiazine hydrochloride as white crystals melting at 180° C and soluble in ethanol and insoluble in water and ether.

WORKUP

后处理

  1. additionwere successively added
  2. temperatureThe mixture was refluxed with agitation for 40 hours
  3. temperatureafter cooling
  4. customthe precipitate formed
  5. customwas removed by vacuum filtration
  6. washThe organic solution was washed with an aqueous solution of sodium bicarbonate
  7. dry with materialwith water, dried
  8. concentrationconcentrated
  9. customThe said product was reacted with an ether solution of hydrogen chloride
  10. filtrationthe obtained precipitate was recovered by vacuum filtration
  11. customwas crystallized from an ethanol ether mixture