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Methanol → HCID 86661429、化合物

HRID 1910382
ノート
印刷プレビュー

反応式

HRID 1910382 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

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

生成物 1

HCID 86661429HCID 86661429、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8df6f06d66ae454cacd1ceeaf017381b
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08603947B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート