Diethyl 2-acetylglutarate → HCID 136067006, Verbindung

HRID 129007

Reaktionsgleichung

Reaktionsgleichung von HRID 129007
CC[O-].[Na+].Cl.[CH3:6][O:7][CH2:8][C:9]([NH2:11])=[NH:10].[C:12]([CH:15]([CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:16](OCC)=[O:17])(=O)[CH3:13]>CCO>[CH3:13][C:12]1[N:11]=[C:9]([CH2:8][O:7][CH3:6])[NH:10][C:16](=[O:17])[C:15]=1[CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24]

Komponenten

5

Edukt 3

HCID 73915Diethyl 2-acetylglutarateHCID 2723922Sodium ethoxideHCID 135486022-Methoxyethanimidamide hydrochloride

Produkt 1

HCID 136067006HCID 136067006, VerbindungAusbeute 42 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of NaOEt (0.088 mol) in EtOH (prepared from 2.0 g of Na and 70 mL of EtOH), methoxyacetamidine hydrochloride (5.4 g, 0.044 mol), and diethyl acetylglutarate (10.0 g, 0.044 mol) was heated under reflux for 24 h. The mixture was concentrated, taken up in water, acidified to pH 4 with conc. HCl, and extracted with CH2Cl2. The extracts were washed with brine, dried (MgSO4), and concentrated. Trituration with ether gave 4.6 g (42%) of product as an off-white solid, mp 87°-90° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 24 h
  3. concentrationThe mixture was concentrated
  4. extractionextracted with CH2Cl2
  5. washThe extracts were washed with brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-2e0daf3a169947c4b577469e4a661227
Quelldatensatz
uspto-grants-1995_11
Patentnummer
US05466692

Verknüpfte Notizen

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