Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Hydrogen iodide | HCID 24841 | — |
| Reactant | 3,6-Dichloro-4,5-dimethylpyridazine | HCID 21187505 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59253660 | HCID 59253660 | 77.5% |
Reaction Steps
A mixture of D9 (0.2 g, 1.13 mmol), sodium iodide (0.420 g, 2.8 mmol) and hydroiodic acid (57 wt. % in water, 2 ml) was stirred at 120° C. for 10 min., under microwave irradiation. The mixture was then poured into an aqueous saturated solution of sodium carbonate, Na2S2O3, water and dichloromethane. The organic phase was separated, filtered over cotton, and the solvent evaporated in vacuo. The residue was purified by column chromatography (dichloromethane/heptane 1:1 to 8:2) to yield D10 (0.235 g, 77%) as a solid. C6H6ClIN2 requires 268. Found 269 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08466153B2 |
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| Source dataset | uspto-grants-2013_06 |
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| ORD ID | ord-b225064bb4114fedbe9f66703f800e39 |
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| Source note | uspto-grants-2013_06 |
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