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Chf-1024 → HCID 19352272, Verbindung

HRID 726889
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 726889
[CH3:1][O:2][C:3]([NH:5][CH:6]1[CH2:15][CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[C:11]([O:18][CH3:19])[C:12]=2[O:16][CH3:17])[C:7]1=O)=[O:4].Cl.OC1C(O)=CC=C2C=1CCC(NC)C2>CO.[Pd]>[CH3:1][O:2][C:3]([NH:5][CH:6]1[CH2:15][CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[C:11]([O:18][CH3:19])[C:12]=2[O:16][CH3:17])[CH2:7]1)=[O:4]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 6918482Chf-1024HCID 19352269HCID 19352269, Verbindung

Produkt 1

HCID 19352272HCID 19352272, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
30 °C

Versuchsvorschrift

50 g of 2-methoxycarbonylamino-5,6-dimethoxy-1-tetralone are dissolved in 500 ml of methanol in a 1000 ml flask, with stirring, 20 g of 5% Pd/C are added, then the whole is placed into an autoclave (Hastelloy) under hydrogen atmosphere at 80° C. and a pressure of 25 atm. for about 6 hours with stirring, after that the mixture is left to cool to about 30° C. in autoclave. The mixture is filtered through Celite and the filtrate is evaporated to dryness under vacuum. The resulting white solid is triturated in 400 ml of n-hexane at 60° C., then is left to cool to about 30° C. with stirring, filtered and dried under vacuum at 60 ° C., to obtain a whitish solid. Yield: 40.6 g, 85.5% (moles), 81.2% (weight); T.L.C. Methylene chloride 95-Methanol 5; Rf=0.76; M.p.=108.7°-111.4 ° C.

Aufarbeitung

  1. stirringa pressure of 25 atm. for about 6 hours with stirring
  2. waitafter that the mixture is left
  3. filtrationThe mixture is filtered through Celite
  4. customthe filtrate is evaporated to dryness under vacuum
  5. customThe resulting white solid is triturated in 400 ml of n-hexane at 60° C.
  6. waitis left
  7. temperatureto cool to about 30° C.
  8. stirringwith stirring
  9. filtrationfiltered
  10. customdried under vacuum at 60 ° C.
  11. customto obtain a whitish solid

Quellen und Nachweise

ORD-Eintrag
ord-060cf77c801f4c2b9ab5e12da8b48f29
Quelldatensatz
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05710336

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