Diethyl (ethoxymethylene)malonate → HCID 59255053, Verbindung

HRID 639537Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 639537
[CH:1]([N:4]=[C:5]([CH3:7])[CH3:6])([CH3:3])[CH3:2].[CH2:8]([O:10][C:11](=[O:22])[C:12](=[CH:18]OCC)[C:13](OCC)=[O:14])[CH3:9]>C1(OC2C=CC=CC=2)C=CC=CC=1>[CH:5]([N:4]1[C:1]([CH3:3])=[CH:2][CH:18]=[C:12]([C:11]([O:10][CH2:8][CH3:9])=[O:22])[C:13]1=[O:14])([CH3:7])[CH3:6]

Komponenten

4

Edukt 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 1378922-Propanamine, N-(1-methylethylidene)-

Produkt 1

HCID 59255053HCID 59255053, VerbindungAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7583Diphenyl EtherLösungsmittel

Reaktionsbedingungen

Temperatur
185 °C

Versuchsvorschrift

A mixture of isopropyl(1-methylethylidene)amine (7.94 g, 80.0 mmol, prepared according to Newcomb, Martin et al., J. Amer. Chem. Soc., 1990, 112, 5186) and diethyl(ethoxymethylene)malonate (17.31 g, 80.0 mmol) in diphenyl ether (48 mL) was stirred in a sealed tube at 180-190° C. for 18 h. After cooling, the mixture was chromatographed on a column of silica gel eluting with n-hexane/ethyl acetate (v/v=1/1˜1/2) to give 12.5 g (70%) of the title compound as brown oil.

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe mixture was chromatographed on a column of silica gel eluting with n-hexane/ethyl acetate (v/v=1/1˜1/2)

Quellen und Nachweise

ORD-Eintrag
ord-fff9c7399a8a4d669d53c55ae152a755
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07691881B2

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