HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiophosgene → HCID 86632901, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiophosgene | HCID 10040 | — |
| Reactant | 6-Methoxy-2-methylpyridin-3-amine | HCID 10290828 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 86632901 | HCID 86632901 | 41% |
Reaction Steps
A mixture of 6-methoxy-2-methylpyridin-3-amine (10.0 g, 0.0724 mol) in tetrahydrofuran (50 mL) and aqueous saturated sodium hydrogen carbonate (50 mL) was added thiophosgene (6.62 mL, 0.0868 mol) at 0° C. The reaction mixture was stirred at room temperature for 1 hr. The mixture was extracted with ethyl acetate (×3). The combined organic layer was washed with brine (×1), dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. To the residue was added n-hexane and the precipitate was removed by filtration and the filtrate was concentrated in vacuo. The residue was washed with cold-n-hexane to give the title compound as a pale yellow solid (5.35 g, 0.0297 mol, 41%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785460B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-0e3d988e72604e9d9c21be96cf86028f |
| Source note | uspto-grants-2014_07 |