HRID253689

反应详情

EQUATION

反应方程式

HRID 253689 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6-(4-bromobutoxy)-indan-1-one prepared by the process described in step (1) above (100 gm, 0.282 mol, 80% purity) and sodium iodide (42 gm, 0.28 mol) in acetonitrile was refluxed for 30 minutes and then cooled to room temperature. 1-(2,3-dichlorophenyl)-piperazine hydrochloride (68 gm, 0.294 mol) and triethyl amine (77 gm, 0.761 mol) were added to the mixture and the resulting mixture was refluxed for 4-6 hr. After solvent was removed, the residue thus obtained was dissolved in chloroform, washed with water which treatment with chloroform and Hydrochloric acid gave 140 g of 6-[4-[4-(2,3-dichlorophenyl)-1-piperazinyl]butoxy]-indan-1-one hydrochloride. This on chloroform solution was basified with ammonium hydroxide to pH 9.5 and extracted with chloroform twice 2×500 ml. The combined chloroform layer was concentrated using rotavapour under reduced pressure to get a residue which on purification with methanol gave 85 gm of 6-[4-[4-(2,3-dichlorophenyl)-1-piperazinyl]-butoxy]-indan-1-one of the formula 2 which has identical characteristic of product obtained for the Example 1, step-2.

WORKUP

后处理

  1. customprepared by the process
  2. temperaturewas refluxed for 30 minutes
  3. temperaturethe resulting mixture was refluxed for 4-6 hr
  4. customAfter solvent was removed
  5. customthe residue thus obtained
  6. washwashed with water which treatment with chloroform and Hydrochloric acid