HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Sulfide → 2,3-Dihydro-5,6-dimethyl-3-thioxo-4-pyridazinecarbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Sulfide | HCID 14804 | — |
| Reactant | 3-chloro-5,6-dimethylpyridazine-4-carbonitrile | HCID 334016 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | 2,3-Dihydro-5,6-dimethyl-3-thioxo-4-pyridazinecarbonitrile | HCID 25648977 | — |
Reaction Steps
A solution of 3-chloro-5,6-dimethylpyridazine-4-carbonitrile (100 mg, 0.60 mmol) and sodium sulfide was stirred in tert-butanol (2.0 mL) in a microwave reaction vial. The vial was sealed and irradiated at 100° C. for 10 minutes. LC/MS indicated product and no remaining starting material. The reaction solution was diluted with IPA (˜10 mL) and stirred at ambient temperature for about 15 minutes, then filtered. The solids on the filter were washed with IPA. The solute was concentrated in vacuo, and the resulting solid was dried overnight at 60° C. in a vacuum oven to give the product. LC/MS: RT=0.24 min., m/z=166 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09056875B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-3fae2a5ebada431f88ff1cc573fdb09b |
| Source note | uspto-grants-2015_06 |