Sodium Chloride → HCID 90387114, Verbindung

HRID 2170229Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2170229
[O:1]=[C:2]([CH3:14])[CH2:3][C:4](ON1C(=O)CCC1=O)=[O:5].[CH3:15][O:16][C:17]1[CH:30]=[CH:29][C:20]([CH2:21][NH:22][CH2:23][CH2:24][C:25]([O:27][CH3:28])=[O:26])=[CH:19][CH:18]=1.C(N(CC)CC)C.[Cl-].[Na+]>ClCCl>[CH3:15][O:16][C:17]1[CH:18]=[CH:19][C:20]([CH2:21][N:22]([CH2:23][CH2:24][C:25]([O:27][CH3:28])=[O:26])[C:4](=[O:5])[CH2:3][C:2](=[O:1])[CH3:14])=[CH:29][CH:30]=1

Komponenten

6

Edukt 4

HCID 5234Sodium ChlorideHCID 8471TriethylamineHCID 5123089N-Hydroxysuccinimidyl acetoacetateHCID 12201326METHYL 3-(4-METHOXYBENZYLAMINO)PROPANOATE

Produkt 1

HCID 90387114HCID 90387114, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A flask with stirbar was charged with 2,5-dioxopyrrolidin-1-yl 3-oxobutanoate (6.47 g, 32.5 mmol), methyl 3-(4-methoxybenzylamino)propanoate (prepared as described in Bew, S. et al, Chem Commun. 2006 (41), 4338-40, 7.7 g, 34.5 mmol) and triethylamine (5 mL, 35.9 mmol) in dichloromethane (125 mL). The solution was stirred overnight at ambient temperature, then shaken in a separatory funnel with saturated aqueous sodium chloride. The organics were then washed with saturated aqueous sodium chloride containing 0.1M HCl and dried over anhydrous sodium sulfate. Filtration and solvent removal provided the title compound.

Aufarbeitung

  1. washThe organics were then washed with saturated aqueous sodium chloride containing 0.1M HCl
  2. dry with materialdried over anhydrous sodium sulfate
  3. filtrationFiltration and solvent removal

Quellen und Nachweise

ORD-Eintrag
ord-29625289c34941ca9a8206d0743ae309
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09050346B2

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