Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 178469927 | HCID 178469927 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67491343 | HCID 67491343 | — |
Reaction Steps
To a solution of ethyl 3-iodo-1H-pyrazole-4-carboxylate (1.10 g, 3.91 mmol) in tert-butanol (5 mL) was added sulfuric acid (0.40 mL, 4.18 mmol, 18 M). The reaction was heated to 100° C. and stirred for 3 hours. The reaction was cooled to room temperature and diluted with ethyl acetate (100 mL) and water (25 mL). The pH was adjusted to 8 with saturated aqueous sodium bicarbonate. The layers were separated and the organics were dried over sodium sulfate, filtered, and concentrated. Purification by flash column chromatography (7-60% ethyl acetate/heptanes) gave 2 regioisomeric products.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08993586B2 |
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| Source dataset | uspto-grants-2015_03 |
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| ORD ID | ord-3fba489d3f0f4d4c9f1198d74043b349 |
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| Source note | uspto-grants-2015_03 |
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