HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → tert-Butyl 3-[4-methyl-6-(4-oxo-4H-1,3-benzothiazin-2-yl)-2-pyridyl]propanoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzoic acid, 2-mercapto-, methyl ester | HCID 21009 | — |
| Reactant | tert-Butyl 3-(6-cyano-4-methyl-2-pyridyl)propanoate | HCID 22939494 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | tert-Butyl 3-[4-methyl-6-(4-oxo-4H-1,3-benzothiazin-2-yl)-2-pyridyl]propanoate | HCID 22939440 | 55% |
Reaction Steps
tert-Butyl 3-(6-cyano-4-methyl-2-pyridyl)propanoate (0.72 g, 2.9 mmol) and methyl thiosalicylate (0.99 g, 5.9 mmol) were dissolved in toluene (4 ml), and triethylamine (2.0 ml, 14.3 mmol) was added thereto. The mixture was refluxed for 14 hrs. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with ethyl acetate-hexane (1:2, v/v) were collected, concentrated and recrystallized from ethyl acetate-hexane to give the titled compound (0.61 g, 54%) as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07767665B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-3e272286012442cfa8d997fd6d7bfac3 |
| Source note | uspto-grants-2010_08 |