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Methanol → HCID 86661429, 화합물

HRID 1910382
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HRID 1910382 반응식
[F:1][C:2]1[C:3]([CH3:18])=[C:4]([CH:8]=[CH:9][C:10]=1[C:11]([F:17])([F:16])[C:12]([F:15])([F:14])[F:13])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:24]O>>[F:1][C:2]1[C:3]([CH3:18])=[C:4]([CH:8]=[CH:9][C:10]=1[C:11]([F:16])([F:17])[C:12]([F:13])([F:14])[F:15])[C:5]([O:7][CH3:24])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 866614303-Fluoro-2-methyl-4-(pentafluoroethyl)benzoic acid

생성물 1

HCID 86661429HCID 86661429, 화합물

실험 절차

2.33 g (8.56 mmol) of 3-fluoro-2-methyl-4-(pentafluoroethyl)benzoic acid were introduced into 30 ml of methanol and admixed with 2 ml of concentrated sulfuric acid. The mixture was subsequently heated at reflux until a check by HPLC indicated full conversion. The contents were freed from the solvent on a rotary evaporator, and the residue was taken up in water. The mixture was extracted twice with ethyl acetate, and the combined organic phases were washed once with saturated aqueous sodium hydrogencarbonate solution. The organic phase was dried and freed from the solvent. The residue obtained was 2.1 g of clean product.

후처리

  1. temperatureThe mixture was subsequently heated
  2. temperatureat reflux until a check by HPLC
  3. customThe contents were freed from the solvent on a rotary evaporator
  4. extractionThe mixture was extracted twice with ethyl acetate
  5. washthe combined organic phases were washed once with saturated aqueous sodium hydrogencarbonate solution
  6. customThe organic phase was dried
  7. customThe residue obtained

출처 및 근거

ORD 기록
ord-8df6f06d66ae454cacd1ceeaf017381b
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08603947B2

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