2,5-Dimethoxytetrahydrofuran → HCID 70532416, Verbindung

HRID 1995322Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1995322
[NH2:1][C:2]1[C:13]2=[C:14]3[N:9]([CH:10]([CH3:15])[CH2:11][CH2:12]2)[CH:8]=[C:7]([C:16]([OH:18])=[O:17])[C:6](=[O:19])[C:5]3=[CH:4][C:3]=1[F:20].CO[CH:23]1[CH2:27][CH2:26][CH:25](OC)O1>C(O)(=O)C>[OH2:17].[F:20][C:3]1[CH:4]=[C:5]2[C:14]3[N:9]([CH:8]=[C:7]([C:16]([OH:18])=[O:17])[C:6]2=[O:19])[CH:10]([CH3:15])[CH2:11][CH2:12][C:13]=3[C:2]=1[N:1]1[CH:23]=[CH:27][CH:26]=[CH:25]1

Komponenten

4

Versuchsvorschrift

To a suspension of 1.0 g of 8-amino-6,7-dihydro-9-fluoro-5-methyl-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid in 20 ml of warm galcial acetic acid was added 1.0 g 2,5-dimethoxytetrahydrofuran. The mixture was heated at reflux for 30 minutes. The product which precipitated was separated by filtration and washed with water to provide yellowish-white crystals of 6,7-dihydro-9-fluoro-5-methyl-1-oxo-8-(1-pyrryl)-1H,5H-benzo[ij]quinolizine-2-carboxylic acid hydrate, m.p. 300° C. Analysis: Calculated for C18H15FN2O3.1/3H2O: %C, 65.0; %H, 4.7; %N, 8.4; Found: %C, 64.8; %H, 4.5; %N, 8.4. The structural assignment was confirmed by infrared and nuclear magnetic resonance spectral analyses.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 30 minutes
  3. customThe product which precipitated
  4. customwas separated by filtration
  5. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-39a70a72e5d649c1b721f29f5c25224c
Quelldatensatz
uspto-grants-1983_09
Patentnummer
US04404207

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