Water → 4-Nitrophenyl isopropyl carbonate

HRID 43279

반응식

HRID 43279 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH2:11](N(CC)CC)C.[C:18]([O:21][CH2:22][CH3:23])(=[O:20])C.O>O1CCCC1.ClC(OC(C)C)=O>[C:18](=[O:20])([O:21][CH:22]([CH3:23])[CH3:11])[O:10][C:7]1[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 9804-NitrophenolHCID 8471TriethylamineHCID 8857Ethyl Acetate

생성물 1

HCID 233903734-Nitrophenyl isopropyl carbonate

시약·촉매·용매 2

HCID 7917Isopropyl chloroformate용매HCID 8028Tetrahydrofuran용매

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.

후처리

  1. temperatureunder cooling on ice
  2. customThe organic layer was separated
  3. washwashed with a saturated sodium chloride aqueous solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customfollowed by solvent removal by evaporation under reduced pressure
  6. dissolutionThe residue was dissolved in 50 mL of ethyl acetate
  7. washwashed with a 5% potassium carbonate aqueous solution
  8. dry with materiala saturated sodium chloride aqueous solution successively and dried over anhydrous magnesium sulfate
  9. customAfter removing the solvent
  10. customby evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-cc3e370ad82d4fa1bf0fa21ad081678d
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536343B2

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