HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chloro-2-sulfanylbenzoic acid → HCID 22939621, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chloro-2-sulfanylbenzoic acid | HCID 20456974 | — |
| Reactant | HCID 22939273 | HCID 22939273 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 22939621 | HCID 22939621 | 19.1% |
Reaction Steps
tert-Butyl 2-(2-cyano-4-pyridyl)ethylcarbamate (1.5 g, 6.0 mmol) and 4-chlorothiosalicylic acid (2.3 g, 12.1 mmol) were dissolved in pyridine (10 ml), and the mixture was refluxed for 18 hrs. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with hexane-ethyl acetate (1:1, v/v) were collected, concentrated and recrystallized from hexane-tetrahydrofuran to give the titled compound (0.48 g, 19%) as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07767665B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-e6d9d706ce9442e89634ca7c0a95a1b9 |
| Source note | uspto-grants-2010_08 |