HRID329050

反应详情

EQUATION

反应方程式

HRID 329050 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.7 g of 2-methylheptanoic acid chloride in 10ml of anhydrous benzene was added dropwise at 10° C to a solution of 6.05 g of 2-trifluoromethyl-10-[3-(4-{2-hydroxyethoxy}-4-methyl-piperidino)-propyl]-phenothiazine in 50 ml of anhydrous benzene containing 1.7 g of triethylamine and the mixture was stirred at room temperature for 20 hours. After washing the benzene solution with water, the mixture was stirred for 4 hours with an aqueous solution saturated with sodium bicarbonate and the organic phase was decanted and concentrated.. The oily residue was purified by chromatography over silica gel with a 99-1 cyclohexane-triethylamine mixture as eluant to obtain 6.5 g of 2-trifluoromethyl-10-[3-(4-{2-methyl -2-heptanoyloxyethoxy}-4-methyl-piperidino)-propyl]-phenothiazine in the form of a yellow oil.

WORKUP

后处理

  1. washAfter washing the benzene solution with water
  2. stirringthe mixture was stirred for 4 hours with an aqueous solution saturated with sodium bicarbonate
  3. customthe organic phase was decanted
  4. concentrationconcentrated
  5. customThe oily residue was purified by chromatography over silica gel with a 99-1 cyclohexane-triethylamine mixture as eluant