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HCID 178418361, Verbindung → HCID 178472446, Verbindung

HRID 1087650
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1087650
[C:1]([O:5][C:6](=[O:44])[CH:7]([CH2:28][N:29](CC1C=CC=CC=1)CC1C=CC=CC=1)[CH2:8][C:9]1([C:14](=[O:27])[NH:15][C@H:16]2[CH2:21][CH2:20][C@@H:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:18][CH2:17]2)[CH2:13][CH2:12][CH2:11][CH2:10]1)([CH3:4])([CH3:3])[CH3:2].[H][H]>C(O)C.[Pd].C(OCC)C>[C:1]([O:5][C:6](=[O:44])[CH:7]([CH2:28][NH2:29])[CH2:8][C:9]1([C:14](=[O:27])[NH:15][C@H:16]2[CH2:17][CH2:18][C@@H:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:20][CH2:21]2)[CH2:13][CH2:12][CH2:11][CH2:10]1)([CH3:3])([CH3:2])[CH3:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 2

HCID 178418361HCID 178418361, VerbindungHCID 178472444HCID 178472444, Verbindung

Produkt 1

HCID 178472446HCID 178472446, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittel
HCID 3283
Diethyl Ether
Lösungsmittel

Versuchsvorschrift

The product from step (c) above (4.6 g, 7.62 mmole) in ethanol (75 ml) was hydrogenated in an atmosphere of hydrogen (50 p.s.i., 3.46 bar) over palladium on charcoal (200 mg), at room temperature overnight. The reaction mixture was filtered through a Solkaflok pad, and the filtrate evaporated to dryness to yield the crude product as an oil. This was dissolved in diethyl ether, and extracted into dilute hydrochloric acid (pH 2) (2x). The combined aqueous layers were washed with diethyl ether, then neutralised with saturated aqueous sodium bicarbonate and extracted with dichloromethane (3x). The combined organic phases were dried (Na2SO4) and evaporated to yield the title amine as an oil (2.91 g, 90%). Found: C,64.80; H,9.28; N,6.76. C23H40N2O5 requires C,65.06; H,9.50; N,6.60%.

Aufarbeitung

  1. filtrationThe reaction mixture was filtered through a Solkaflok pad
  2. customthe filtrate evaporated to dryness
  3. customto yield the crude product as an oil
  4. extractionextracted into dilute hydrochloric acid (pH 2) (2x)
  5. washThe combined aqueous layers were washed with diethyl ether
  6. extractionextracted with dichloromethane (3x)
  7. dry with materialThe combined organic phases were dried (Na2SO4)
  8. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-c65f2719c31d4b579371d2fe80bfacad
Quelldatensatz
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05036104

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