HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 68552826, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | tert-Butyl (3-oxo-3-phenylpropyl)carbamate | HCID 17818960 | — |
| Reactant | HCID 78358145 | HCID 78358145 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 68552826 | HCID 68552826 | — |
Reaction Steps
To a cooled (0° C.) solution of tert-butyl 3-oxo-3-phenylpropylcarbamate (0.68 g, 2.73 mmol) and 2,5-difluorobenzothiohydrazide hydrochloride (0.613 g, 2.73 mmol) in EtOH (27 mL) was added triethylamine (0.57 mL, 4.09 mmol). After stirring at room temperature for 8 hours, the mixture was heated to 65° C. for 16 hours. The mixture was concentrated under reduced pressure and the residue was dissolved in ethyl acetate (100 mL). The solution was washed with water and brine (40 mL), dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was chromatographed (30% ethyl acetate in hexanes) to provide the crude product as a brown syrup which was used directly in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08324257B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-c63fc19e878f4ca095abbc1fc082e9e3 |
| Source note | uspto-grants-2012_12 |