Benzylamine → HCID 22903655, Verbindung

HRID 1489157Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1489157
ON1C2C=CC=CC=2N=N1.C1(N=C=NC2CCCCC2)CCCCC1.[CH2:26]([N:33]1[C:37](=[O:38])[CH2:36][C:35]([C:44]([O-:46])=O)([C:39]([O:41][CH2:42][CH3:43])=[O:40])[CH2:34]1)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1.[CH2:47]([NH2:54])[C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=1>O1CCCC1>[CH2:26]([N:33]1[C:37](=[O:38])[CH2:36][C:35]([C:44](=[O:46])[NH:54][CH2:47][C:48]2[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=2)([C:39]([O:41][CH2:42][CH3:43])=[O:40])[CH2:34]1)[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1

Komponenten

6

Edukt 4

HCID 7504BenzylamineHCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 86751384HCID 86751384, Verbindung

Produkt 1

HCID 22903655HCID 22903655, VerbindungAusbeute 99,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

1-Hydroxybenztriazole (2.78 g) and dicyclohexylcarbodiimide (42.5 g) were added to a mixture of monoethyl 1-benzyl-5-oxopyrrolidine-3,3-dicarboxylate (60.0 g), benzylamine (23.2 g) and tetrahydrofuran (500 ml), and the mixture was stirred at room temperature overnight. The insoluble matter was removed by filtration and the filtrate was concentrated. Ethyl acetate (400 ml) was added and the mixture was sequentially washed with an aqueous solution of potassium carbonate, water, dilute hydrochloric acid and saturated brine, dried, and concentrated to give 78 g of the object compound as white crystals, melting point 63°-65° C.

Aufarbeitung

  1. customThe insoluble matter was removed by filtration
  2. concentrationthe filtrate was concentrated
  3. additionEthyl acetate (400 ml) was added
  4. washthe mixture was sequentially washed with an aqueous solution of potassium carbonate, water, dilute hydrochloric acid and saturated brine
  5. customdried
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-4a379a635a0b4a66bb9f12e491c00d19
Quelldatensatz
uspto-grants-1997_10
Patentnummer
US05677316

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