反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe solution was cooled
- customthe solvent evaporated
- additionthe residue treated with water
- extractionThe product was extracted with chloroform
- washwashed with water
- dry with materialdried (MgSO4)
- customEvaporation
- customgave a gum which
- filtrationThe crystallised solid was collected by filtration
- dissolutiondissolved in ethanol
- additiontreated with ethanolic HCl
- additionEther was added
- filtrationthe resulting precipitate filtered off
- customrecrystallised from isopropyl alcohol