反应详情

In a 20 ml-three necked flask, 0.013 g of lithium chloride and 3.8 ml of DMF were placed. To the mixture, a solution of 1.09 g (6.22 mM) of 4-butylphenyl isocyanate and 6.20 mM of optically active 4-methoxystyrene oxide in 1.3 ml of DMF was added dropwise in 12 minutes under refluxing and stirring in nitrogen atmosphere, followed by refluxing for 50 minutes under stirring. After the reaction, the reaction mixture was left standing for cooling, then poured into water, and subjected to extraction with ethyl acetate. The organic layer was washed with water, dried with anhydrous sodium sulfate and evaporated under reduced pressure to obtain a residue The residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=10/1) and recrystallized from methanol to obtain 0.29 g of optically active 3-(4-butylphenyl)-5-(4-methoxyphenyl)-2-oxazolidinone (Yield: 14.5%).

1. temperatureunder refluxing
2. temperatureby refluxing for 50 minutes
3. stirringunder stirring
4. customAfter the reaction
5. waitthe reaction mixture was left
6. temperaturefor cooling
7. extractionsubjected to extraction with ethyl acetate
8. washThe organic layer was washed with water
9. dry with materialdried with anhydrous sodium sulfate
10. customevaporated under reduced pressure
11. customto obtain a residue The residue
12. customwas purified by silica gel column chromatography (eluent: toluene/ethyl acetate=10/1)
13. customrecrystallized from methanol