HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Azidobutyrophenone → 2-(3-Azidopropyl)-5-(2,5-difluorophenyl)-2-phenyl-2,3-dihydro-1,3,4-thiadiazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Azidobutyrophenone | HCID 10877918 | — |
| Reactant | Benzenecarbothioic acid, 2,5-difluoro-, hydrazide | HCID 55279024 | — |
| Catalyst | Acetic Acid | HCID 176 | — |
| Solvent | Dichloromethane ethanol | HCID 21584144 | — |
| Product | 2-(3-Azidopropyl)-5-(2,5-difluorophenyl)-2-phenyl-2,3-dihydro-1,3,4-thiadiazole | HCID 86604831 | 54.7% |
Reaction Steps
To a solution of 2,5-difluorobenzothiohydrazide (1.5 g, 7.97 mmol) in EtOH/dichloromethane (3:1, 16 mL) was added 4-azido-1-phenylbutan-1-one (1.36 g, 7.17 mmol). After stirring at room temperature for 16 hours, acetic acid (2 drops) was added and the mixture was stirred for another 16 hours. The reaction mixture was then concentrated under reduced pressure and chromatographed (9:1 hexanes/ethyl acetate) to provide the product (1.41 g, 41%) as a bright yellow syrup.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07449486B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-439b96e1a6b34328bbae7de376cfb7d2 |
| Source note | uspto-grants-2008_11 |