p-Toluenesulfonic acid monohydrate → HCID 67868427, Verbindung

HRID 467289Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 467289
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10]1[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][C:11]=1[CH2:17][C:18]([OH:20])=[O:19].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[C:18]([OH:20])(=[O:19])[CH3:17].[CH3:17][C:11]1[CH:12]=[C:13]([OH:16])[CH:14]=[CH:15][C:10]=1[NH:9][C:3]1[C:4]([Cl:8])=[CH:5][CH:6]=[CH:7][C:2]=1[Cl:1]

Komponenten

4

Edukt 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 30525665-Hydroxydiclofenac

Produkt 1

HCID 67868427HCID 67868427, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of the acid of Step E, above (2.0 g, 6.4 mmol) in 20 mL of methanol containing a few mg of p-toluene sulfonic acid monohydrate is heated at reflux for 3 hours. The solvent is evaporated in vacuo and the residue dissolved in ethyl acetate. The organic phase is washed with saturated NaHCO3, brine and dried (MgSO4). Removal of solvent affords the product (1.9 g, 90%) as a brown foam. It is used as such in the next step.

Aufarbeitung

  1. temperatureat reflux for 3 hours
  2. customThe solvent is evaporated in vacuo
  3. dissolutionthe residue dissolved in ethyl acetate
  4. washThe organic phase is washed with saturated NaHCO3, brine
  5. dry with materialdried (MgSO4)
  6. customRemoval of solvent

Quellen und Nachweise

ORD-Eintrag
ord-320cad30f9e642d0981bd5322cbbd22a
Quelldatensatz
uspto-grants-1992_10
Patentnummer
US05159085

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