p-Toluenesulfonic acid → Methyl 3-benzoylbenzoate

HRID 332688

反応式

HRID 332688 の反応式
[C:1]([C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12]([OH:14])=[O:13])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:18]C1C=CC(S(O)(=O)=O)=CC=1>CO>[C:1]([C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12]([O:14][CH3:18])=[O:13])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 1013863-Benzoylbenzoic acid

生成物 1

HCID 349621Methyl 3-benzoylbenzoate収率 905.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A stirred solution of 3-benzoylbenzoic acid (10.0 g, 44.4 mmol) and p-TSA (0.85 g, 4.39 mmol) in methanol (200 mL) was heated at 75° C. for 18 hours. The reaction mixture was allowed to cool, and the solvent evaporated at reduced pressure. The residue was partitioned between ethyl acetate and saturated aqueous sodium hydrogen carbonate. The organic phase was dried with anhydrous sodium sulfate, filtered, and the filtrate was evaporated at reduced pressure to afford the title compound (9.55 g, 90%).

後処理

  1. temperatureto cool
  2. customthe solvent evaporated at reduced pressure
  3. customThe residue was partitioned between ethyl acetate and saturated aqueous sodium hydrogen carbonate
  4. dry with materialThe organic phase was dried with anhydrous sodium sulfate
  5. filtrationfiltered
  6. customthe filtrate was evaporated at reduced pressure

出典と根拠

ORDレコード
ord-d39238a40f694b9b81a0d9f53718ff8e
出典データセット
uspto-grants-2014_11
特許番号
US08877774B2

関連ノート

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