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Ethanol → HCID 59314223, Verbindung

HRID 1047916
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1047916
[CH2:1]([O:3][C:4]([C:6]1([C:15](=[O:27])[NH:16][C:17]2[CH:26]=[CH:25][CH:24]=[C:23]3[C:18]=2[CH:19]=[CH:20][N:21]=[CH:22]3)[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)=[O:5])[CH3:2].CCO>[Pt](=O)=O.C(O)(=O)C>[CH2:1]([O:3][C:4]([C:6]1([C:15](=[O:27])[NH:16][C:17]2[CH:26]=[CH:25][CH:24]=[C:23]3[C:18]=2[CH2:19][CH2:20][NH:21][CH2:22]3)[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)=[O:5])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 702EthanolHCID 59314243HCID 59314243, Verbindung

Produkt 1

HCID 59314223HCID 59314223, VerbindungAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 345198Adams' catalystKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A 100 mL Parr reaction vessel is charged with 2-(Isoquinolin-5-ylcarbamoyl)-indan-2-carboxylic acid ethyl ester (320, 500 mg, 1.39 mmol) and EtOH (10 mL). The reaction vessel is agitated by swirling until dissolution ° C. curred. Acetic acid (10 mL) and platinum (IV) oxide (117 mg, 0.52 mmol) are added. The vessel is fitted on a Parr hydrogenation apparatus, flushed with N2 and then evacuated. The vessel is charged with hydrogen to 50 psi. The apparatus is set to agitate. After 4 h, agitation is ceased. The reaction vessel is evacuated and flushed with nitrogen. This process is repeated. The contents of the reaction vessel are diluted with iPrOH (50 mL) and filtered through a pad of celite. Solvent is removed from the filtrate under reduced pressure. The resulting residue is reconstituted in iPrOH (15 mL) and toluene (15 mL). The solvent is removed under reduced pressure. This process is repeated. Pumping to constant weight yields light beige solid (0.5 g, 99%).

Aufarbeitung

  1. customA 100 mL Parr reaction vessel
  2. dissolutionby swirling until dissolution ° C
  3. customThe vessel is fitted on a Parr hydrogenation apparatus
  4. customflushed with N2
  5. customevacuated
  6. additionThe vessel is charged with hydrogen to 50 psi
  7. stirringto agitate
  8. customThe reaction vessel is evacuated
  9. customflushed with nitrogen
  10. additionThe contents of the reaction vessel are diluted with iPrOH (50 mL)
  11. filtrationfiltered through a pad of celite
  12. customSolvent is removed from the filtrate under reduced pressure
  13. customThe solvent is removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-03cd3320d718463899a00bc0e72f1aae
Quelldatensatz
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08569535B2

Notizen zur Reaktion

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