Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl isocyanate | HCID 8022 | — |
| Reactant | HCID 67498744 | HCID 67498744 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67499248 | HCID 67499248 | 95.9% |
Reaction Steps
To a solution of 3-methyl-1-(pyridin-3-yl)-1H-pyrazol-4-amine (0.1 g, 0.574 mmol) in DCM (5.74 ml) was added ethyl isocyanate (0.041 g, 0.574 mmol) and the reaction mixture was stirred at ambient temperature for 40 minutes. The reaction mixture had turned from a clear solution to a suspension with white solid material. The reaction mixture was concentrated and purified using silica gel chromatography (0-20% MeOH/DCM) to yield the title compound as a white solid (0.135 g, 95%): mp 197-200° C.; 1H NMR (400 MHz, CDCl3) δ 8.94 (d, J=2.3 Hz, 1H), 8.48-8.37 (m, 1H), 8.32 (s, 1H), 7.94 (d, J=8.3 Hz, 1H), 7.52 (br s, 1H), 7.41-7.25 (m, 1H), 5.79 (br s, 1H), 3.33-3.23 (m, 2H), 2.29 (d, J=2.9 Hz, 3H), 1.16 (dd, J=8.7, 5.7 Hz, 3H); ESIMS m/z 246 ([M+H]+), 244 ([M−H]−).
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-7ea36733a7ba47aeb8e506266b7b0708 |
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| Source note | uspto-grants-2014_08 |
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