Acetic Acid → HCID 69003844, Verbindung

HRID 225511Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 225511
CO[CH2:3][CH2:4][O:5][CH3:6].[C:7](/[C:9](/[C:24]1[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=1)=[CH:10]\[N:11]([CH2:19][C:20]([O:22][CH3:23])=[O:21])CCC(OCC)=O)#[N:8].[CH2:30]1[CH2:40]CN2C(=NCCC2)CC1.C(O)(=[O:43])C>>[NH2:8][C:7]1[C:9]([C:24]2[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=2)=[C:10]([CH2:40][CH2:30][C:6]([O:5][CH2:4][CH3:3])=[O:43])[NH:11][C:19]=1[C:20]([O:22][CH3:23])=[O:21]

Komponenten

5

Edukt 4

HCID 176Acetic AcidHCID 80711,2-DimethoxyethaneHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 23122145HCID 23122145, Verbindung

Produkt 1

HCID 69003844HCID 69003844, VerbindungAusbeute 70 %

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To an ethylene glycol dimethyl ether (50 mL) solution of ethyl 3-{((1Z)-2-cyano-2-(3-pyridyl)vinyl)[(methoxycarbonyl)methyl]amino}propanate (6.236 g) was added 1,8-diazabicyclo[5,4,0]-7-undecene (3.590 g), and the mixture was stirred at 60° C. overnight. The reaction solution was cooled to room temperature and neutralized with acetic acid, and the solvent was distilled off under reduced pressure. The residue was purified by column chromatography on silica gel (hexane/ethyl acetate=1/5), to obtain the title compound (4.380 g, yield 70%). The NMR data and ESI/MS data of the compound are given below.

Aufarbeitung

  1. distillationthe solvent was distilled off under reduced pressure
  2. customThe residue was purified by column chromatography on silica gel (hexane/ethyl acetate=1/5)

Quellen und Nachweise

ORD-Eintrag
ord-41352add16f3403abe5a7a49ecec2673
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07557113B2

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