HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → tert-Butyl (6-(4-Oxo-4H-1,3-benzothiazin-2-yl)-2-pyridyl]methylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzoic acid, 2-mercapto-, methyl ester | HCID 21009 | — |
| Reactant | tert-Butyl 6-cyano-2-pyridylmethylcarbamate | HCID 22939432 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | tert-Butyl (6-(4-Oxo-4H-1,3-benzothiazin-2-yl)-2-pyridyl]methylcarbamate | HCID 59750386 | 72% |
Reaction Steps
tert-Butyl (6-cyano-2-pyridyl)methylcarbamate (1.6 g, 6.8 mmol) and methyl thiosalicylate (1.8 g, 10.9 mmol) were dissolved in toluene (6 ml), and triethylamine (3.0 ml, 21.5 mmol) was added thereto. The mixture was refluxed for 20 hrs. After cooling, the precipitates were collected by filtration and dissolved in chloroform. The solution was subjected to a silica gel column chromatography. The fractions eluted with chloroform-methanol (20:1, v/v) were collected, concentrated and recrystallized from hexane-chloroform to give the titled compound (1.8 g, 72%) as pale yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07767665B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-199fe2f7b6134c3db314c233bfdbb1fe |
| Source note | uspto-grants-2010_08 |