Reaktion #521876

Reaktionsgleichung

9-chloro-8-fluoro-2-methyl-1,2-dihydro-6-oxo-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid

thiomorpholine

→

9-thiomorpholino-8-fluoro-2-methyl-1,2-dihydro-6-oxo-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid

Ausbeute 8.9%

Lösungsmittel

hexamethylphosphoric triamide

hexamethylphosphoric triamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas reacted at 150° C. for 7 hours
2. 2
   workup.DISTILLATIONwas distilled off under reduced pressure
3. 3
   Sonstigethe residue was recrystallized from dimethylformamide

Vorschrift

A mixture of 28 g of 9-chloro-8-fluoro-2-methyl-1,2-dihydro-6-oxo-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid, 5 g of thiomorpholine and 30 ml of hexamethylphosphoric triamide in a stainless steel autoclave was reacted at 150° C. for 7 hours. After completion of reaction, hexamethylphosphoric triamide was distilled off under reduced pressure and the residue was recrystallized from dimethylformamide to give 1.5 g of 9-thiomorpholino-8-fluoro-2-methyl-1,2-dihydro-6-oxo-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid. m.p. not lower than 300° C., slightly yellow rhombic crystals.

Quelle