Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 15814132 | HCID 15814132 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18999869 | HCID 18999869 | — |
Reaction Steps
To an ice-colded suspension of NaH (0.062 g) in 20 ml of anhydrous THF under N2 is added 7-(5-chlorothien-2-yl)-1H-pyrazolo[3,4-g]quinoxaline (0.63 g). The orange-red mixture is stirred at the same temperature for 5 minutes, then iodomethane (0.374 g) is added dropwise to the orange-red mixture. The resulting mixture is stirred at room temperature overnight, then poured into water, extracted with methylene chloride, separated, dried (MeSO4), concentrated in vacuo to give a yellow solid. Purification is by chromatography eluting first with 5% ethylacetate in hexane, then gradually up to 30% ethylacetate in hexane to isolate 1-methyl-7-(5-chlorothien-2-yl)-1H-pyrazolo[3,4-g]quinoxaline (m.p. 225°-227° C.), then up to 10% hexane in ethylacetate to isolate 2-methyl-7-(5-chlorothien-2-yl)-2H-pyrazolo[3,4-g]quinoxaline (m.p. 222°-224° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05476851 |
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| Source dataset | uspto-grants-1995_12 |
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| ORD ID | ord-36dd87bb1e064b9aa788eb6dd6d23fa3 |
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| Source note | uspto-grants-1995_12 |
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