Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3-Methyl-2(1H)-pyridinethione | HCID 5371450 | — |
| Reactant | HCID 67485726 | HCID 67485726 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67487618 | HCID 67487618 | 60.8% |
Reaction Steps
3-Methylpyridine-2(1H)-thione (0.906 g, 7.24 mmol) and 5-bromo-3-(2-methylpyridin-3-yloxy)picolinonitrile (2.00 g, 6.89 mmol) were dissolved in DMF (12 mL) and the mixture was cooled to 0° C. Sodium hydride (95%; 0.183 g, 7.24 mmol) was slowly added and the reaction was warmed to ambient temperature and stirred overnight. The reaction mixture was poured into water (100 mL), stirred for 30 minutes, then filtered to afford a solid which was purified over silica gel (2:3 hexanes:ethyl acetate). Concentration of the second UV active fraction to elute afforded 5-(3-methylpyridin-2-ylthio)-3-(2-methylpyridin-3-yloxy)picolinonitrile (1.40 g, 4.19 mmol, 60.7% yield) as a pale yellow/off white powder/crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08853409B2 |
|---|
| Source dataset | uspto-grants-2014_10 |
|---|
| ORD ID | ord-4b34118769014acf8391293851713d42 |
|---|
| Source note | uspto-grants-2014_10 |
|---|