Water → 2-Methoxy-5-(4-nitrophenoxy)benzoic acid

HRID 598437노트

반응식

HRID 598437 반응식
C[O:2][C:3]([C:5]1[CH:6]=[C:7]([CH:18]=[CH:19][C:20]=1[O:21][CH3:22])[O:8][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][CH:10]=1)=[O:4].[OH-].[K+].O>CO>[C:3]([C:5]1[CH:6]=[C:7]([CH:18]=[CH:19][C:20]=1[O:21][CH3:22])[O:8][C:9]1[CH:10]=[CH:11][C:12]([N+:15]([O-:17])=[O:16])=[CH:13][CH:14]=1)([OH:4])=[O:2]

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 230230954-(3-Methoxycarbonyl-4-methoxyphenoxy)-1-nitrobenzene

생성물 1

HCID 230230632-Methoxy-5-(4-nitrophenoxy)benzoic acid수율 90.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 4-(3-methoxycarbonyl-4-methoxyphenoxy)-1-nitrobenzene (1.2 g), KOH (0.33 g) and water (5 mL) in MeOH (45 mL) was stirred at room temp. overnight and then heated at the reflux temp. for 4 h. The resulting mixture was cooled to room temp. and concentrated under reduced pressure. The residue was dissolved in water (50 mL), and the aqueous mixture was made acidic with a 1N HCl solution. The resulting mixture was extracted with EtOAc (50 mL). The organic layer was dried (MgSO4) and concentrated under reduced pressure to give 4-(3-carboxy-4-methoxyphenoxy)-1-nitrobenzene (1.04 g).

후처리

  1. temperatureheated at the reflux temp
  2. waitfor 4 h
  3. temperatureThe resulting mixture was cooled to room temp.
  4. concentrationconcentrated under reduced pressure
  5. dissolutionThe residue was dissolved in water (50 mL)
  6. extractionThe resulting mixture was extracted with EtOAc (50 mL)
  7. dry with materialThe organic layer was dried (MgSO4)
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-86a2916fb9114c2aac2b1c53f972024a
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897623B2

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