HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → N'-(2-fluoro-4-nitro-thiobenzoyl)hydrazinecarboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | N'-(2-fluoro-4-nitrobenzoyl)hydrazinecarboxylic acid tert-butyl ester | HCID 68487050 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | N'-(2-fluoro-4-nitro-thiobenzoyl)hydrazinecarboxylic acid tert-butyl ester | HCID 86610078 | 110.3% |
Reaction Steps
N′-(2-Fluoro-4-nitro-benzoyl)hydrazinecarboxylic acid tert-butyl ester (Step 1, 2.32 g, 7.75 mmol) and Lawesson's reagent (2.35 g, 5.81 mmol) in dioxane (50 ml) are heated at 85° C. overnight. The mixture is evaporated under vacuum and the residue purified by flash column chromatography (70% dichloromethane/hexane) to give the title compound as a bright orange solid (2.02 g, 82%), [M+H]+=316.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06919329B2 |
| Source dataset | uspto-grants-2005_07 |
| ORD ID | ord-8e7d59ecca2f48d0961d1b270a9ffd95 |
| Source note | uspto-grants-2005_07 |