4-Nitrophenol → Methyl (4-nitrophenoxy)acetate

HRID 83778노트

반응식

HRID 83778 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].C([O-])([O-])=O.[K+].[K+].Cl[CH2:18][C:19]([O:21][CH3:22])=[O:20]>CC(C)=O>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:18][C:19]([O:21][CH3:22])=[O:20])=[CH:6][CH:5]=1)([O-:3])=[O:2]

참가 물질

5

반응물 3

HCID 9804-NitrophenolHCID 7295Methyl chloroacetateHCID 11430Potassium Carbonate

생성물 1

HCID 700522Methyl (4-nitrophenoxy)acetate수율 72.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a mixture of 4-nitrophenol (100 g, 719 mmol) and anhydrous K2CO3 (400 gm, 2.894 mol) in anhydrous acetone (950 ml) was added methyl chloroacetate (114 g, 1.050 moles) and refluxed for 12 hours. Acetone was distilled off and water (1500 ml) was added. Crude 7 was filtered, dried and recrystallised from a mixture of ethyl acetate:hexane (1:5) to give pure 7 (110 g, 72.5%) as a white fluffy powder with an m.p between 97-98.4° C.

후처리

  1. temperaturerefluxed for 12 hours
  2. distillationAcetone was distilled off
  3. additionwater (1500 ml) was added
  4. filtrationCrude 7 was filtered
  5. customdried
  6. customrecrystallised from a mixture of ethyl acetate:hexane (1:5)

출처 및 근거

ORD 기록
ord-babbe404bc1e4121af8d645fddc011eb
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846845B2

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