HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 18772052, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Ethyl bromopyruvate | HCID 66144 | — |
| Reactant | 2,6-dichloropyridine-4-carbothioamide | HCID 2781859 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 18772052 | HCID 18772052 | — |
Reaction Steps
2,6-Dichloropyridine-4-thiocarboxamide (1.0 g, 4.83 mmol) was dissolved in dry 1,4-dioxane followed by adding ethyl bromopyruvate (0.9 mL, 7.24 mmol) and pyridine (0.4 mL, 4.83 mmol). The resulting mixture was heated to reflux under N2 for 5 h. After cooling to RT, solvent was removed. The residue was extracted with CHCl3. The organic layer was washed with H2O and brine, dried over MgSO4, and concentrated to give a brownish solid. This crude was purified by chromatography on silica gel. Elution with hexane:acetone (90:10) gave a title compound as yellow solid. MS m/z: 303 (M+H). Calc'd. for C11H8Cl2N2O2S-303.16.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07196104B2 |
| Source dataset | uspto-grants-2007_03 |
| ORD ID | ord-b0e3719767fa48b58aeb12e2ec3ebe5c |
| Source note | uspto-grants-2007_03 |