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Sodium Bicarbonate → HCID 15380923, Verbindung

HRID 610773
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 610773
[CH:1]1([NH:7][C:8](=[O:32])[CH2:9][CH2:10][CH2:11][CH2:12][N:13](CC2C=CC=CC=2)[CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[O:23][CH3:24])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(=O)([O-])O.[Na+]>C(O)(=O)C.ClCCl.[Pd]>[CH:1]1([NH:7][C:8](=[O:32])[CH2:9][CH2:10][CH2:11][CH2:12][NH:13][CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[O:23][CH3:24])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 2

HCID 516892Sodium BicarbonateHCID 15380922HCID 15380922, Verbindung

Produkt 1

HCID 15380923HCID 15380923, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23938PalladiumKatalysatorHCID 176Acetic AcidLösungsmittelHCID 6344Dichloromethane
Lösungsmittel

Versuchsvorschrift

A catalyst composed of palladium on 10% moist carbon (1.5 g) is added to a solution of N-cyclohexyl-5-[benzyl{2-(2-methoxyphenoxy)ethyl}amino]pentan-amide (3 g, 6.8 mmole) in glacial acetic acid (30 ml) and the mixture is hydrogenated for 2 hours at 20° C. The catalyst is removed by filtration and the solvent is evaporated under reduced pressure. The residue obtained in the form of a salt of acetic acid is taken up in dichloromethane (50 ml) and the base is liberated by treatment with a saturated solution of sodium hydrogen carbonate. The organic phase is collected, washed with water, dried over magnesium sulfate and the solvent is evaporated under reduced pressure. The expected product is obtained in the form of a white powder after crystallisation in diethylether (0.95 g, 40%).

Aufarbeitung

  1. customThe catalyst is removed by filtration
  2. customthe solvent is evaporated under reduced pressure
  3. customThe residue obtained in the form of a salt of acetic acid
  4. customThe organic phase is collected
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate
  7. customthe solvent is evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-29b105d75a934ead962d7185fd212f04
Quelldatensatz
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05998666

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