Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 22097002 | HCID 22097002 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 22097040 | HCID 22097040 | 89% |
Reaction Steps
A 1:1 mixture of the two isomers of N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-N-(1 -methoxycarbonyl- 1-ethyl)-methanesulphonamide (Preparation 23, 1.40 g, 32 mmol), 2M hydrochloric acid (40 ml) and dioxane (40 ml) was heated in an autoclave at 130° C. for 48 h and 150° C. for 24 h. The mixture was cooled, concentrated to low volume under reduced pressure and the solid filtered off and washed with ether. The product was dissolved in 1M aqueous sodium hydroxide (40 ml) and precipitated by the addition of 2M hydrochloric acid (to pH3). The white solid was filtered off and dried in vacuo, to give the title compound (1.13 g, 89%), as a mixture of diastereomers, m.p. 282° C. (dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05852016 |
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| Source dataset | uspto-grants-1998_12 |
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| ORD ID | ord-979669467829439995022db94c9aa8b7 |
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| Source note | uspto-grants-1998_12 |
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