反応 #94836

反応方程式

1-(1,4-Benzodioxan-2-yl)-2-bromoethanol

2-(piperid-4-yl)-1,2-benzisothiazolin-3-one-1,1-dioxide hydrochloride

triethylamine

→

title compound

2-([2-(1,4-benzodioxan-2-yl)-2-hydroxyethyl]piperid-4-yl)-1,2-benzoisothiazolin-3-one-1,1-dioxide

溶媒

isopropyl alcohol

ethanol

反応条件

後処理

1. 1
   温度The solution was cooled
2. 2
   その他the solvent evaporated
3. 3
   workup.ADDITIONthe residue treated with water
4. 4
   抽出The product was extracted with chloroform
5. 5
   洗浄washed with water
6. 6
   乾燥dried (MgSO4)
7. 7
   その他Evaporation
8. 8
   その他gave a gum which
9. 9
   ろ過The crystallised solid was collected by filtration
10. 10
    workup.DISSOLUTIONdissolved in ethanol
11. 11
    workup.ADDITIONtreated with ethanolic HCl
12. 12
    workup.ADDITIONEther was added
13. 13
    ろ過the resulting precipitate filtered off
14. 14
    その他recrystallised from isopropyl alcohol

実験手順

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.

出典