ChemicalBook CAS DataBase List Licostinel

Licostinel synthesis

9synthesis methods

Product Name:Licostinel
CAS Number:153504-81-5
Molecular formula:C8H3Cl2N3O4
Molecular Weight:276.03

25983-13-5 Synthesis

6,7-DICHLORO-1,4-DIHYDRO-2,3-QUINOXALINEDIONE

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Yield:-

Reaction Conditions:

in conc. H₂ SO₄;

Steps:

1.B Method B

This product was used in the next reaction without further purification. 5-Nitro-6,7-dichloro-1,4-dihydroquinoxaline-2,3-dione: 3.335 g (14.5 mmol) of 6,7-dichloro-1,4-dihydroquinoxaline-2,3-dione was dissolved in 65 mL of conc. H₂ SO₄ with stirring and cooling in an ice-H₂ O bath, then 2.20 g (21.76 mmol) of KNO₃ (Baker, used as received) was added in portions over 10 min. with stirring. The resulting mixture was stirred at 22° C. under N₂ for 20 h. then was slowly poured into ice-H₂ O (400 mL) with stirring. The precipitate was collected on a sintered funnel by vacuum filtration, washed with H₂ O (5*10 mL), and dried at 60° C. under 0.1 mmHg for 12 h affording 3.39 g (85%) of the crude 6,7-dichloro-5-nitro-1,4-dihydroquinoxaline-2,3-dione as a grey-yellow powder. Purity: >98.5% based on HPLC analysis.

References:

US5514680,1996,A