Ethanol → Ethyl 2',4'-Difluoro-4-hydroxy[1,1'-biphenyl]-3-carboxylate

HRID 85396

反応式

HRID 85396 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[C:11]([C:16]([OH:18])=[O:17])[CH:10]=1.[CH2:19](O)[CH3:20]>S(=O)(=O)(O)O>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[C:11]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:10]=1

参加物

4

反応物 2

HCID 702EthanolHCID 3059Diflunisal

生成物 1

HCID 23078331Ethyl 2',4'-Difluoro-4-hydroxy[1,1'-biphenyl]-3-carboxylate

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
80 °C

実験手順

2′,4′-difluoro-4-hydroxybiphenyl-3-carboxylic acid (1.0 g, 4.0 mmol) was dissolved in ethanol (30 mL) and sulfuric acid (8 mL). The solution was stirred (80° C., 18 h) and then concentrated under reduced pressure. The residue was dissolved in ethyl acetate and washed with water, brine and dried over MgSO4. Solvent evaporation afforded ethyl 2′,4′-difluoro-4-hydroxybiphenyl-3-carboxylate (1.0 g). Mass calculated for C15H12F2O3=278.25; found: [M+H]+=279.1.

後処理

  1. concentrationconcentrated under reduced pressure
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with water, brine
  4. dry with materialdried over MgSO4
  5. customSolvent evaporation

出典と根拠

ORDレコード
ord-a286ace1d6794b16b595376991b025a4
出典データセット
uspto-grants-2014_09
特許番号
US08846972B2

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