Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Fuming sulfuric acid | HCID 24681 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 86757459 | HCID 86757459 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 21696676 | HCID 21696676 | — |
Reaction Steps
Methyl 3,6-dichloropyridine-2-carboxylate N-oxide (5.0 g, 22.52 mmol) was dissolved in a minimum amount of H2SO4. The mixture was cooled in an ice/water bath and to it was slowly added 30% oleum (9.6 mL) and fuming HNO3 (9.6 mL), gradually heated to 65° C. and stirred for 48 hr. The cooled reaction mixture was diluted with ethyl acetate (200 mL) and to it was carefully added saturated sodium bicarbonate. The product was extracted with ethyl acetate (2×150 mL) and the combined extracts were dried (MgSO4) and concentrated to give 0.10 g of a yellow solid; mp 192-193° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06297197B1 |
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| Source dataset | uspto-grants-2001_10 |
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| ORD ID | ord-b7278315d1144850911926697803a758 |
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| Source note | uspto-grants-2001_10 |
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