Licostinel synthesis
- Product Name:Licostinel
- CAS Number:153504-81-5
- Molecular formula:C8H3Cl2N3O4
- Molecular Weight:276.03
25983-13-5
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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
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