HRID847435

反应详情

EQUATION

反应方程式

HRID 847435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Hydroxyphenyl methanol (124 g, 1 mole) and 192 g (1 mole) of 1-(2-methoxyphenyl)piperazine, together with 56 g (1 mole) of potassium hydroxide and 8.7 g (0.1 mole) of lithium bromide and 32.2 g (0.1 mole) of Aliquat 366 were dissolved in a mixture of 1 liter of toluene and 1 liter of water. The reaction mixture was refluxed for 24 hours, and then allowed to cool to room temperature. The organic layer was decanted and extracted twice with 500 ml of a 10% sodium hydroxide solution. The basic aqueous liquor was treated with ammonium acetate to provoke precipitation of the desired product. After filtration and drying under vacuum overnight at 50° C., 167 g (0.56 mole, 56% yield) of the title product was obtained as small white leaflets melting at 172° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 24 hours
  2. customThe organic layer was decanted
  3. extractionextracted twice with 500 ml of a 10% sodium hydroxide solution
  4. additionThe basic aqueous liquor was treated with ammonium acetate
  5. customprecipitation of the desired product
  6. filtrationAfter filtration
  7. customdrying under vacuum overnight at 50° C.