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HCID 18536675, Verbindung → HCID 18536678, Verbindung

HRID 412046
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 412046
[CH2:1]([O:3][CH:4]([O:12][CH2:13][CH3:14])[C:5](=O)[CH:6]([CH3:10])[C:7](=O)[CH3:8])[CH3:2].C(=O)(O)[O-].[C:19]1([NH:25][C:26]([NH2:28])=[NH2+:27])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C(O)C>[CH3:10][C:6]1[C:5]([CH:4]([O:12][CH2:13][CH3:14])[O:3][CH2:1][CH3:2])=[N:27][C:26]([NH:25][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:28][C:7]=1[CH3:8]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 18536675HCID 18536675, VerbindungHCID 178512436HCID 178512436, Verbindung

Produkt 1

HCID 18536678HCID 18536678, VerbindungAusbeute 114,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

A mixture of 44 g (purity about 50%, about 0.11 mol) of 1,1-diethoxy-3-methylpentane-2,4-dione (crude product, Example 2a) and 35 g (0.175 mol) of phenylguanidinium bicarbonate in 300 ml of ethanol was heated at 70-80° C. for about 3 hours. The reaction mixture was then concentrated and the residue was filtered, with suction, through silica gel using methyl tert-butyl ether. The solvent was evaporated. Less volatile components were distilled off under a pressure of 0.3 mbar, at a bath temperature of 150° C. The residue obtained was 38 g (quantitative yield) of the title compound as a yellow oil.

Aufarbeitung

  1. concentrationThe reaction mixture was then concentrated
  2. filtrationthe residue was filtered, with suction, through silica gel
  3. customThe solvent was evaporated
  4. distillationLess volatile components were distilled off under a pressure of 0.3 mbar, at a bath temperature of 150° C
  5. customThe residue obtained

Quellen und Nachweise

ORD-Eintrag
ord-f34b6f5bfc144fff828b8d7d3e3917ff
Quelldatensatz
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06562833B1

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