Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| Reactant | HCID 10388243 | HCID 10388243 | — |
| Reactant | HCID 20071503 | HCID 20071503 | — |
| Solvent | Benzene | HCID 241 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178472041 | HCID 178472041 | 41.7% |
Reaction Steps
In 5 ml of benzene was dissolved 500 mg of ethyl 4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5-trifluorobenzoylacetate. To the resulting solution was added 411 mg of N,N-dimethylformamide-dimethylacetal, and the resulting mixture was refluxed for 40 minutes. The reaction mixture was concentrated under reduced pressure, and the residue obtained was dissolved in 5 ml of ethanol. To the resulting solution were added 157 mg of 2-aminothioethanol hydrochloride and 139 mg of triethylamine, and the resulting mixture was stirred at room temperature for 16 hours. The reaction mixture was concentrated under reduced pressure and the residue obtained was purified by a column chromatography (eluant: toluene/ethyl acetate=5/1) to obtain 250 mg (yield: 41.7%) of ethyl 2-[4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5-trifluorobenzoyl]-3-(2-mercaptoethylamino)acrylate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04990508 |
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| Source dataset | uspto-grants-1991_02 |
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| ORD ID | ord-d6c81e89ff914b39af83a0b3cfe84d52 |
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| Source note | uspto-grants-1991_02 |
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