反応 #1345128

反応方程式

(4-(6-Propyldecahydronaphthalene-2-yl)cyclohexyl)methyl p-toluenesulfonate

4-Ethoxy-2,3-difluorophenol

potassium carbonate

→

2-(4-((4-ethoxy-2,3-difluorophenoxy)methyl)cyclohexyl)-6-propyldecahydronaphthalene

収率 59.7%

溶媒

DMF

反応条件

後処理

1. 1
   洗浄The reaction mixture was washed with water
2. 2
   乾燥dried over anhydrous magnesium sulfate
3. 3
   workup.DISTILLATIONThe DMF was distilled off under reduced pressure
4. 4
   その他The residue was purified by silica gel column chromatography (eluent: ethyl acetate/n-heptane=1/20 by volume)
5. 5
   その他by recrystallization (solvent: Solmix/n-heptane=1/4 by volume)

実験手順

(4-(6-Propyldecahydronaphthalene-2-yl)cyclohexyl)methyl p-toluenesulfonate (3.5 g) prepared in the tenth step was dissolved in DMF (50 ml). 4-Ethoxy-2,3-difluorophenol (1.6 g) and potassium carbonate (2.2 g) were added, and the mixture was stirred at 70° C. for 5 hours. The reaction mixture was washed with water, and dried over anhydrous magnesium sulfate. The DMF was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: ethyl acetate/n-heptane=1/20 by volume) and then by recrystallization (solvent: Solmix/n-heptane=1/4 by volume) to give 2-(4-((4-ethoxy-2,3-difluorophenoxy)methyl)cyclohexyl)-6-propyldecahydronaphthalene (2.1 g).

出典