HRID66558

反应详情

EQUATION

反应方程式

HRID 66558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Erythro 1-(1,4-Benzodioxan-2-yl)-2-bromoethanol (1.29 g, 0.005 m), 2-(piperid-4-yl)-1,2-benzisothiazolin-3-one-1,1-dioxide hydrochloride (1.44 g, 0.005 m) and triethylamine (4 cm3) were refluxed for 24 hours in ethanol (50 cm3). The solution was cooled, the solvent evaporated and the residue treated with water. The product was extracted with chloroform, washed with water and dried (MgSO4). Evaporation gave a gum which was dissolved in isopropyl alcohol. The crystallised solid was collected by filtration, dissolved in ethanol and treated with ethanolic HCl. Ether was added and the resulting precipitate filtered off and recrystallised from isopropyl alcohol to give the title compound as the hydrochloride salt, m.p. 216°-218° C.

WORKUP

后处理

  1. temperatureThe solution was cooled
  2. customthe solvent evaporated
  3. additionthe residue treated with water
  4. extractionThe product was extracted with chloroform
  5. washwashed with water
  6. dry with materialdried (MgSO4)
  7. customEvaporation
  8. customgave a gum which
  9. filtrationThe crystallised solid was collected by filtration
  10. dissolutiondissolved in ethanol
  11. additiontreated with ethanolic HCl
  12. additionEther was added
  13. filtrationthe resulting precipitate filtered off
  14. customrecrystallised from isopropyl alcohol