Dimethylformamide → HCID 22440208, Verbindung

HRID 963256

Reaktionsgleichung

Reaktionsgleichung von HRID 963256
Cl[C:2]1[C:11]2[CH:10]=[C:9]([OH:12])[CH:8]=[CH:7][C:6]=2[N:5]=[C:4]2[C:13]3[C:18]([C:19](=[O:20])[C:3]=12)=[CH:17][CH:16]=[CH:15][CH:14]=3.C(=O)([O-])[O-].[Li+].[Li+].Cl.[CH2:28]([N:30]([CH2:34]C)[CH2:31][CH2:32][SH:33])C.CN(C)C=O>O>[CH3:28][N:30]([CH2:31][CH2:32][S:33][C:2]1[C:11]2[CH:10]=[C:9]([OH:12])[CH:8]=[CH:7][C:6]=2[N:5]=[C:4]2[C:13]3[C:18]([C:19](=[O:20])[C:3]=12)=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH3:34]

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 11125Lithium CarbonateHCID 16031Ethanethiol, 2-(diethylamino)-, hydrochloride (1:1)HCID 19081815HCID 19081815, Verbindung

Produkt 1

HCID 22440208HCID 22440208, VerbindungAusbeute 63,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

A mixture of 400 mg (1.4 mmol) of 10-chloro-8-hydroxy-11H-indeno[1,2-b]quinolin-11-one, 629 mg (8.5 mmol) of lithium carbonate, 963 mg (5.7 mmol) of 2-diethylaminoethanethiol hydrochloride and 8 ml of N,N-dimethylformamide was stirred for 5 hours with heating at 90° C. After completion of the reaction, the reaction mixture was added to water, and precipitated crystals were collected by filteration. The crystals were recrystallized from ethanol, giving 310 mg of the title compound (yield: 57.7%). The property values are shown in Table 1.

Aufarbeitung

  1. customAfter completion of the reaction
  2. customprecipitated crystals
  3. customwere collected by filteration
  4. customThe crystals were recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-f77d3e454a19410ba31af60dc53a8981
Quelldatensatz
uspto-grants-1998_06
Patentnummer
US05763453

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