HRID2082361

反应详情

EQUATION

反应方程式

HRID 2082361 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.1 g of N-piperid-4-yl-N-methylpropionamide acetate, 90 ml of dimethylformamide and 6.3 ml of triethylamine are introduced into a 250 ml three-necked flask. 6.6 g of 2,3-dihydro-2-iodomethylbenzofuran are poured onto the mixture which is heated to 60°-65° C. This temperature is maintained for 15 hours. The reaction mixture is evaporated to dryness and the residue is taken up in ethyl acetate and extracted with 150 ml of N hydrochloric acid. The aqueous phase is rendered alkaline with sodium hydroxide in the presence of ethyl acetate. The organic phase is washed with water and dried over magnesium sulphate. The solvent is evaporated to yield a base in the form of a brown oil, which is converted into a salt with 3.8N ethereal hydrogen chloride to yield the desired compound.

WORKUP

后处理

  1. temperatureis heated to 60°-65° C
  2. temperatureThis temperature is maintained for 15 hours
  3. customThe reaction mixture is evaporated to dryness
  4. extractionextracted with 150 ml of N hydrochloric acid
  5. washThe organic phase is washed with water
  6. dry with materialdried over magnesium sulphate
  7. customThe solvent is evaporated
  8. customto yield a base in the form of a brown oil, which