반응 #42023

반응 방정식

4-(3-bromopropylthio)-2-hydroxy-3-propylphenyl-ethanone

ethyl 4-(6-acetyl-3-hydroxy-2-propylphenoxy)butyrate

potassium iodide

potassium carbonate

→

title compound

ethyl 4-[6-acetyl-3-[3-(4-acetyl-3-hydroxy-2-propylphenylthio)-propoxy]-2-propyl phenoxy]butyrate

용매

acetone

acetone

반응 조건

후처리

1. 1
   온도with heating to reflux
2. 2
   온도After refluxing six hours the mixture
3. 3
   기타inorganic materials were separated by filtration
4. 4
   농축The filtrate was concentrated
5. 5
   기타the residue was separated
6. 6
   기타purified by silica-gel column chromatography (eluting with benzene:ethyl acetate=9:1)

실험 절차

To a stirred mixture of ethyl 4-(6-acetyl-3-hydroxy-2-propylphenoxy)butyrate (1.6 g), potassium iodide (0.5 g) and potassium carbonate (1.45 g) in acetone (30 ml) was added drop wise a solution of 4-(3-bromopropylthio)-2-hydroxy-3-propylphenyl-ethanone (1.9 g) in acetone (10 ml) with heating to reflux. After refluxing six hours the mixture was cooled to room temperature and inorganic materials were separated by filtration. The filtrate was concentrated and the residue was separated and purified by silica-gel column chromatography (eluting with benzene:ethyl acetate=9:1) to give the title compound as crude crystals (2.1 g, 72.4%) which were recrystallized from ethanol to give colorless crystals, mp 65-66° C.

출처