p-Toluenesulfonic acid monohydrate → HCID 86720817, Verbindung

HRID 2205695

Reaktionsgleichung

Reaktionsgleichung von HRID 2205695
[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

Komponenten

4

Edukt 2

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

Produkt 1

HCID 86720817HCID 86720817, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-3b09d947aa8f40c78ef32dcc3aff60ad
Quelldatensatz
uspto-grants-2016_06
Patentnummer
US09371318B2

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