p-Toluenesulfonic acid monohydrate → HCID 86720817、化合物

HRID 2205695

反応式

HRID 2205695 の反応式
[CH3:1][O:2][CH:3]=[CH:4][C:5]1[CH:14]=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[CH:7][CH:6]=1.[OH2:15].[C:16]1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[CH3:16][O:15][CH:3]([O:2][CH3:1])[CH2:4][C:5]1[CH:14]=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[CH:7][CH:6]=1

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 54136641Methyl 4-(2-methoxyethenyl)benzoate

生成物 1

HCID 86720817HCID 86720817、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of methyl 4-(2-methoxyvinyl)benzoate (1.36 g, 7.08 mmol) in methanol (30 mL) was added para-toluenesulfonic acid monohydrate (pTSA) (0.135 g, 0.71 mmol) and the reaction mixture heated under reflux for 18 hours. The solvent was evaporated at reduced pressure. The residue was partitioned between DCM and 10% aqueous potassium carbonate. The organic phase was poured through a hydrophobic frit and the solvent evaporated at reduced pressure. The crude material was used in the next step without further purification.

後処理

  1. temperaturethe reaction mixture heated
  2. temperatureunder reflux for 18 hours
  3. customThe solvent was evaporated at reduced pressure
  4. customThe residue was partitioned between DCM and 10% aqueous potassium carbonate
  5. additionThe organic phase was poured through a hydrophobic frit
  6. customthe solvent evaporated at reduced pressure
  7. customThe crude material was used in the next step without further purification

出典と根拠

ORDレコード
ord-3b09d947aa8f40c78ef32dcc3aff60ad
出典データセット
uspto-grants-2016_06
特許番号
US09371318B2

関連ノート

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