Hydrazine hydrate (1:1) → HCID 22011014, Verbindung

HRID 323151Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 323151
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:49]=[CH:48][C:20]([C:21]([N:23]([CH3:47])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[O:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][N:36]4C(=O)C5=CC=CC=C5C4=O)=[O:22])=[CH:19][CH:18]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:4][CH:3]=1.O.NN>C(O)C.C(OCC)C>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:18]=[CH:19][C:20]([C:21]([N:23]([CH3:47])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[O:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][NH2:36])=[O:22])=[CH:48][CH:49]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:6][CH:7]=1

Komponenten

5

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 22010690HCID 22010690, Verbindung

Produkt 1

HCID 22011014HCID 22011014, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A suspension of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-(5-phthalimidopentyloxy)phenyl]benzamide (1.1 g) in ethanol (20 ml) was stirred rapidly and treated with hydrazine hydrate (844 mg). The mixture was stirred at 60° C. for 3 hours. After cooling, the reaction mixture was diluted with diethyl ether and filtered through Celite. The Celite was washed with diethyl ether, and the filtrate was concentrated. The residual milky oil was again dissolved in diethyl ether, filtered through Celite, washed with diethyl ether, and concentrated to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-(5-aminopentyloxy)phenyl]benzamide

Aufarbeitung

  1. stirringThe mixture was stirred at 60° C. for 3 hours
  2. temperatureAfter cooling
  3. filtrationfiltered through Celite
  4. washThe Celite was washed with diethyl ether
  5. concentrationthe filtrate was concentrated
  6. dissolutionThe residual milky oil was again dissolved in diethyl ether
  7. filtrationfiltered through Celite
  8. washwashed with diethyl ether
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-49c9de55c9e049e1a499f8bc0666c42d
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06211242B1

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