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Methanol → Methyl 5-fluoro-2-iodobenzoate

HRID 1971832
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HRID 1971832 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([I:11])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].OS(O)(=O)=O.[OH-].[Na+].[CH3:19]O>>[CH3:19][O:8][C:7](=[O:9])[C:6]1[CH:10]=[C:2]([F:1])[CH:3]=[CH:4][C:5]=1[I:11]
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참가 물질

5

반응물 4

HCID 887MethanolHCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 131585835-Fluoro-2-iodobenzoic acid

생성물 1

HCID 53486126Methyl 5-fluoro-2-iodobenzoate수율 98%

실험 절차

A mixture of 5-fluoro-2-iodo-benzoic acid (10.05 g, 39.47 mmol) and conc. H2SO4 (10 mL) in MeOH (100 ml) was reflux for 6 hours. After cooling to room temperature, NaOH (2N) was added dropwise to adjust the pH˜8. After most of organic solvent was removed under reduced pressure, the mixture was extracted with dichloromethane three times. The combined organic layers were washed with water, dried and concentrated to give the titled compound (10.80 g, yield 98%)

후처리

  1. temperaturewas reflux for 6 hours
  2. customAfter most of organic solvent was removed under reduced pressure
  3. extractionthe mixture was extracted with dichloromethane three times
  4. washThe combined organic layers were washed with water
  5. customdried
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b809cd07a3684f20b019cadc15329a29
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08431581B2

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