HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetophenone → HCID 68503997, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetophenone | HCID 7410 | — |
| Reactant | Benzenecarbothioic acid, 2,5-difluoro-, hydrazide | HCID 55279024 | — |
| Solvent | Dichloromethane ethanol | HCID 21584144 | — |
| Product | HCID 68503997 | HCID 68503997 | 70.3% |
Reaction Steps
To a solution of acetophenone (0.600 g, 5.00 mmol) in 20 mL of a 3:1 EtOH/DCM mixture was added 2,5-difluorobenzothiohydrazide (0.941 g, 5.00 mmol). The reaction was allowed to stir overnight at room temperature. The reaction was then heated to 45° C., for 14 hours. The reaction mixture was then concentrated in vacuo, and the residue was loaded directly to Biotage (45), followed by flash column chromatography (20% ethyl acetate/hexanes), yielding 5-(2,5—the desired product (1.021 g, 70% yield) as a yellow semi-solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08268871B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-2c66f6bf98644d4488bcc46e8b35b88f |
| Source note | uspto-grants-2012_09 |