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HCID 22975755, Verbindung → HCID 22975754, Verbindung

HRID 1860283
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1860283
[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][CH2:8][N:9]2[CH2:14][CH2:13][C:12]3([CH2:19][CH2:18][CH:17]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:16][CH2:15]3)[CH2:11][CH2:10]2)=[CH:3][CH:2]=1>C(O)(=O)C.[Pt](=O)=O>[NH:1]1[CH2:2][CH2:3][CH:4]([CH2:7][CH2:8][N:9]2[CH2:14][CH2:13][C:12]3([CH2:15][CH2:16][CH:17]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:18][CH2:19]3)[CH2:11][CH2:10]2)[CH2:5][CH2:6]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 1

HCID 22975755HCID 22975755, Verbindung

Produkt 1

HCID 22975754HCID 22975754, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 345198Adams' catalystKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

0.17 g (0.5 mmol) of the compound from Example 22 were dissolved in 25 ml 90% acetic acid followed by addition of 30 mg platinum(IV) oxide. The mixture was filled into an autoclave and hydrogenated for 4 h at room temperature and a pressure of 20 atm. The catalyst was removed by filtration and the solvent evaporated under reduced pressure. The residue was treated with water and neutralized with sodium carbonate followed by extraction with dichloromethane. The organic layer was dried over sodium sulfate and concentrated in vacuo to leave the pure title compound.

Aufarbeitung

  1. additionThe mixture was filled into an autoclave and hydrogenated for 4 h at room temperature
  2. customThe catalyst was removed by filtration
  3. customthe solvent evaporated under reduced pressure
  4. additionThe residue was treated with water and neutralized with sodium carbonate
  5. extractionfollowed by extraction with dichloromethane
  6. dry with materialThe organic layer was dried over sodium sulfate
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-1ae32dc774e54c008036d00fe30f0877
Quelldatensatz
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06528534B2

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