反応 #61881

反応方程式

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

溶媒

acetone

acetone

反応条件

後処理

1. 1
   温度with heating to reflux
2. 2
   温度After refluxing six hours the mixture
3. 3
   その他inorganic materials were separated by filtration
4. 4
   濃縮The filtrate was concentrated
5. 5
   その他the residue was separated
6. 6
   その他purified by silica-gel column chromatography (eluting with benzene:ethyl acetate=9:1)

実験手順

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.

出典