HCID 69766304, Verbindung → HCID 10404453, Verbindung

HRID 966106Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 966106
Cl.[OH:2][C:3]1[C:4]([O:24][CH3:25])=[C:5]([C:10](=[O:23])[CH2:11][NH:12][C:13]([CH3:22])([CH3:21])[CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:6]=[CH:7][C:8]=1[OH:9]>CO.[Pt](=O)=O>[CH3:22][C:13]([NH:12][CH2:11][CH:10]([C:5]1[C:4]([O:24][CH3:25])=[C:3]([OH:2])[C:8]([OH:9])=[CH:7][CH:6]=1)[OH:23])([CH3:21])[CH2:14][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

Komponenten

4

Edukt 1

HCID 69766304HCID 69766304, Verbindung

Produkt 1

HCID 10404453HCID 10404453, VerbindungAusbeute 64,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 345198Adams' catalystKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

10 g of 1-(3,4-dihydroxy-2-methoxyphenyl)-2-(1,1-dimethyl-2-phenylethylamino)ethanone hydrochloride is hydrogenated with 0.5 g of platinum(IV) oxide in 200 mL methanol. The catalyst is suction filtered and the solvent is distilled off under reduced pressure. The residue remaining is dissolved in 200 mL acetonitrile, combined with 5 g of sodium benzoate and refluxed for 15 minutes. After the excess sodium benzoate has been filtered off, the product which crystallizes out of the filtrate is filtered off and washed with acetonitrile and diethyl ether. Yield: 64.5% (benzoate); melting point: 149° C.-150° C.

Aufarbeitung

  1. filtrationfiltered
  2. distillationthe solvent is distilled off under reduced pressure
  3. dissolutionThe residue remaining is dissolved in 200 mL acetonitrile
  4. temperaturerefluxed for 15 minutes
  5. filtrationAfter the excess sodium benzoate has been filtered off
  6. customthe product which crystallizes out of the filtrate
  7. filtrationis filtered off
  8. washwashed with acetonitrile and diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-8914d004eec047e09517829430d632a7
Quelldatensatz
uspto-grants-2005_10
Patentnummer
US06951888B2

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