Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 136375618 | HCID 136375618 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 135712889 | HCID 135712889 | 81.3% |
Reaction Steps
7-Phenyl-2-thioxo-2,3-dihydropyrazolo[1,5-a][1,3,5]triazin-4(1H-one (6.4 g, 26.2 mmol) was dissolved in absolute ethanol (150 mL). To this solution was added aqueous sodium hydroxide (2.1 g, 53 mmol in 50 mL of water) and finally iodomethane (1.7 mL, 27.3 mmol) was added dropwise. The resulting solution was stirred at room temperature for 3 hours and then concentrated to a white solid. This solid was suspended in water and the mixture acidified (to pH=1) with concentrated sulfuric acid. The resulting precipitate was collected by filtration, washed with water and dried to give 2-(methylsulfanyl)-7-phenylpyrazolo[1,5-a][1,3,5]triazin-4(3H)-one (5.5 g, 81%) as a white solid. 1H-NMR (DMSO-d6): δ 7.99 (d, 2H), 7.5 (m, 3H), 6.93 (s, 1H), 2.58 (s, 3H); MS m/z 259 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07247626B2 |
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| Source dataset | uspto-grants-2007_07 |
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| ORD ID | ord-ed1d04dc64ae484aabbc95ae30bfb46b |
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| Source note | uspto-grants-2007_07 |
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