HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium methanethiolate → HCID 54276775, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium methanethiolate | HCID 4378561 | — |
| Reactant | 2,6-Dibromo-4-nitropyridine | HCID 16038748 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 54276775 | HCID 54276775 | 85.1% |
Reaction Steps
To a solution of 2,6-dibromo-4-nitro-pyridine (CAS 175422-04-5, 10.0 g, 35.5 mmol) in 60 mL of DMF was added at −10° C. sodium methanethiolate (2.61 g, 1.05 eq.) and the mixture stirred for 45 Min. at this temperature and for another 2 h at 0° C. Pouring onto crashed ice, twofold extraction with AcOEt, washing with water and brine, drying over magnesium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, hexane/AcOEt=97/3), yielded 8.55 g of the title compound as off-white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08163778B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-1b732ba545f14fdc99dde1ea72e1c2b3 |
| Source note | uspto-grants-2012_04 |