Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | O-Xylene | HCID 7237 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | 4-Fluoro-3-methoxyacetamidobenzoic acid | HCID 18412417 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 18412295 | HCID 18412295 | — |
Reaction Steps
A mixture of 3.0 g (11.7 mmol) of 4-fluoro-3-methoxyacetamidobenzoic acid and 2.1 g (5.2 mmol) of Lawesson's reagent was refluxed for 6 hours in 90 ml toluene, mixed with 1.0 g Lawesson's reagent and heated to 120° C. for another 6 hours. After the solvent was replaced with xylene, the mixture was heated to 180° C. for a further 8 hours in a pressurised vessel. Then the solvent was distilled off in vacuo, the crude product obtained was purified by flash chromatography (silica gel; ethyl acetate/petroleum ether=5:95), and evaporated down again.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06414008B1 |
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| Source dataset | uspto-grants-2002_07 |
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| ORD ID | ord-efbc0689973849c5ac1e0872ced6a152 |
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| Source note | uspto-grants-2002_07 |
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