HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Methyl-2-sulfanylbenzoic acid → tert-Butyl 6-(8-methyl-4-oxo-4H-1,3-benzothiazin-2-yl)-2-pyridinecarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Methyl-2-sulfanylbenzoic acid | HCID 12612808 | — |
| Reactant | tert-Butyl 6-cyanopicolinate | HCID 22939377 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | tert-Butyl 6-(8-methyl-4-oxo-4H-1,3-benzothiazin-2-yl)-2-pyridinecarboxylate | HCID 22939413 | 58.3% |
Reaction Steps
tert-Butyl 6-cyano-2-pyridinecarboxylate (3.2 g, 15 mmol) and 3-methylthiosalicylic acid (4.7 g, 28 mmol) were dissolved in pyridine (40 ml), and the mixture was refluxed for 16 hrs. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with hexane-tetrahydrofuran (2:1, v/v) were collected, concentrated and recrystallized from hexane-tetrahydrofuran to give the titled compound (3.1 g, 56%) 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-b052ffc30c134d6aa4a02440c773f99c |
| Source note | uspto-grants-2010_08 |