반응 #71557

반응 방정식

4-nitrophenol

triethylamine

ethyl acetate

water

→

4-nitrophenyl isopropyl carbonate

용매

tetrahydrofuran

isopropyl chloroformate

반응 조건

후처리

1. 1
   온도under cooling on ice
2. 2
   기타The organic layer was separated
3. 3
   세척washed with a saturated sodium chloride aqueous solution
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   기타followed by solvent removal by evaporation under reduced pressure
6. 6
   workup.DISSOLUTIONThe residue was dissolved in 50 mL of ethyl acetate
7. 7
   세척washed with a 5% potassium carbonate aqueous solution
8. 8
   건조a saturated sodium chloride aqueous solution successively and dried over anhydrous magnesium sulfate
9. 9
   기타After removing the solvent
10. 10
    기타by evaporation under reduced pressure

실험 절차

Into a solution of 3.00 g of 4-nitrophenol and 3.31 mL of triethylamine in 30 mL of tetrahydrofuran, 2.46 mL of isopropyl chloroformate was dropped under cooling on ice. To the reaction mixture, after stirred at the same temperature for 10 min, ethyl acetate and water were added. The organic layer was separated, washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate, followed by solvent removal by evaporation under reduced pressure. The residue was dissolved in 50 mL of ethyl acetate, washed with a 5% potassium carbonate aqueous solution and a saturated sodium chloride aqueous solution successively and dried over anhydrous magnesium sulfate. After removing the solvent by evaporation under reduced pressure, 3.00 g of 4-nitrophenyl isopropyl carbonate was obtained as a light yellow solid.

출처