HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 10712381, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | 3,3,3-Trifluoro-2-hydroxy-2-methylpropanoic acid | HCID 2775125 | — |
| Reactant | HCID 15814262 | HCID 15814262 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 10712381 | HCID 10712381 | — |
Reaction Steps
Thionyl chloride (110 μl, 1.51 mmol) is added to 3,3,3-trifluoro-2-hydroxy-2-methylpropanoic acid (240 mg, 1.52 mmol) in 5 ml of N,N-dimethylacetamide at -15°/-10° C., and the mixture is stirred at this temperature for one hour. Then 2-amino-5-(phenylcarbonyl) thiophene (200 mg, 0.983 mmol) is added and the reaction mixture is equilibrated to room temperature. After the reaction has ended, the reaction mixture is poured into 200 ml of water and subjected to extraction with 3×100 ml of ethyl acetate. The combined organic phases are dried over magnesium sulfate and filtered and the solvent is distilled off. The orange-colored oil which remains is purified by flash chromatography (eluent: 50% v/v ethyl acetate in petroleum ether (40/60)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05627198 |
| Source dataset | uspto-grants-1997_05 |
| ORD ID | ord-b0fbcdd9471e4e3aa3c61ffa1e84eb09 |
| Source note | uspto-grants-1997_05 |