تفاعل #71557

ord-cc3e370ad82d4fa1bf0fa21ad081678d

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةunder cooling on ice
  2. 2
    أخرىThe organic layer was separated
  3. 3
    غسيلwashed with a saturated sodium chloride aqueous solution
  4. 4
    تجفيفdried over anhydrous magnesium sulfate
  5. 5
    أخرىfollowed by solvent removal by evaporation under reduced pressure
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in 50 mL of ethyl acetate
  7. 7
    غسيلwashed with a 5% potassium carbonate aqueous solution
  8. 8
    تجفيفa saturated sodium chloride aqueous solution successively and dried over anhydrous magnesium sulfate
  9. 9
    أخرىAfter removing the solvent
  10. 10
    أخرىby evaporation under reduced pressure

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08536343B2uspto-grants-2013_09