Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3-Fluoropyridine | HCID 67794 | — |
| Reactant | HCID 178428694 | HCID 178428694 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67499429 | HCID 67499429 | 51.2% |
| Product | HCID 67499863 | HCID 67499863 | 6% |
Reaction Steps
To a solution of 3-methyl-1H-pyrazole (10.99 g, 134 mmol) in N,N-dimethylformamide (100 ml) at 0° C. was added sodium hydride (3.71 g, 154 mmol, 60% dispersion). The reaction was stirred at 0° C. for 2 hours. 3-Fluoropyridine (10.0 g, 103 mmol) was added, and the reaction was stirred at 100° C. overnight. The reaction was cooled to room temperature and water was added slowly. The mixture was extracted with dichloromethane and the combined organic phases were washed with brine, concentrated and chromatographed (0-100% ethyl acetate/hexanes) to afford 3-(3-methyl-1H-pyrazol-1-yl)pyridine (8.4 g, 52.77 mmol, 51.2%) and 3-(5-methyl-1H-pyrazol-1-yl)pyridine (1.0 g, 6%). Analytical data of both products is consistent with that reported under Example 6, Step 1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08815271B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-d9fcfe94c6f94eec8517ae4c8ffe81fc |
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| Source note | uspto-grants-2014_08 |
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