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Methanol → Methyl 2-(3-methoxy-4-nitrophenyl)acetate

HRID 1019749
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HRID 1019749 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:12][C:13]([OH:15])=[O:14])[CH:6]=[CH:7][C:8]=1[N+:9]([O-:11])=[O:10].[CH3:16]O>OS(O)(=O)=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:12][C:13]([O:15][CH3:16])=[O:14])[CH:6]=[CH:7][C:8]=1[N+:9]([O-:11])=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 887MethanolHCID 16755859(3-Methoxy-4-nitrophenyl)acetic acid

생성물 1

HCID 67467853Methyl 2-(3-methoxy-4-nitrophenyl)acetate수율 92%

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

실험 절차

A solution of 2-(3-methoxy-4-nitrophenyl)acetic acid (4.6 g, 21.78 mmol) and concentrated H2SO4 (2 drops) in methanol (200 mL) was heated to reflux for 3 hours. The mixture was allowed to cool to room temperature then the solvents were removed under reduced pressure. The residue was partitioned between water (100 mL) and EtOAc (100 mL), then the separated organic layer was washed with sodium bicarbonate solution (100 mL), brine (200 mL), dried (Na2SO4) and evaporated under reduced pressure to give the title compound (4.5 g, 92%) as a solid.

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후처리

  1. temperatureto reflux for 3 hours
  2. customthe solvents were removed under reduced pressure
  3. customThe residue was partitioned between water (100 mL) and EtOAc (100 mL)
  4. washthe separated organic layer was washed with sodium bicarbonate solution (100 mL), brine (200 mL)
  5. dry with materialdried (Na2SO4)
  6. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b89fb5257c694111a67f4d04bceac5a5
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716287B2

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