Methanol → Methyl 2-(4-(cyclopropanecarbonyl)phenyl)acetate

HRID 1838688노트

반응식

HRID 1838688 반응식
[CH:1]1([C:4]([C:6]2[CH:11]=[CH:10][C:9]([CH2:12][C:13]([OH:15])=[O:14])=[CH:8][CH:7]=2)=[O:5])[CH2:3][CH2:2]1.[CH3:16]O>S(=O)(=O)(O)O>[CH:1]1([C:4]([C:6]2[CH:11]=[CH:10][C:9]([CH2:12][C:13]([O:15][CH3:16])=[O:14])=[CH:8][CH:7]=2)=[O:5])[CH2:2][CH2:3]1

참가 물질

4

반응물 2

HCID 887MethanolHCID 1937314-(Cyclopropylcarbonyl)benzeneacetic acid

생성물 1

HCID 12096482Methyl 2-(4-(cyclopropanecarbonyl)phenyl)acetate수율 68%

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

실험 절차

Dissolve 4-(cyclopropylcarbonyl)benzeneacetic acid in methanol (100 mL) containing concentrated sulfuric acid (10 drops). Stir 24 hours. Add triethylamine (2 mL) and concentrate the solution. Dissolve the residue in water/ethyl acetate. Wash the organic phase with saturated sodium hydrogen carbonate solution, dry over anhydrous magnesium sulfate and concentrate. Purify by silica gel chromatography (400 mL silica gel, 20% ethyl acetate/heptane as eluent) to give the title compound (4.6 g, 68%).

후처리

  1. concentrationAdd triethylamine (2 mL) and concentrate the solution
  2. dissolutionDissolve the residue in water/ethyl acetate
  3. washWash the organic phase with saturated sodium hydrogen carbonate solution
  4. dry with materialdry over anhydrous magnesium sulfate
  5. concentrationconcentrate
  6. customPurify by silica gel chromatography (400 mL silica gel, 20% ethyl acetate/heptane as eluent)

출처 및 근거

ORD 기록
ord-5b79177fec8746d6b951758c36f9f45c
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06673933B2

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