p-Toluenesulfonic acid monohydrate → HCID 86720817、化合物

HRID 877317

反応式

HRID 877317 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 fit 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 fit
  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-b56a5c9f0c3648a4ab4d0770ff57f6d0
出典データセット
uspto-grants-2015_03
特許番号
US08987299B2

関連ノート

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