HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9951743, 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 19956158 | HCID 19956158 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 9951743 | HCID 9951743 | — |
Reaction Steps
Thionyl chloride (80 μl, 1.1 mmol) is added to 3,3,3-trifluoro-2-hydroxy-2-methylpropanoic acid (170 mg, 1.08 mmol) in 5 ml of N,N-dimethylacetamide at -15°/-10° C. and the mixture is stirred at this temperature for one hour. After adding 2-amino-5-(phenylsulfonyl)thiophene (170 mg, 0.710 mmol) and equilibration to room temperature and 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-753c202fbc094e6aad64ce763f1282d0 |
| Source note | uspto-grants-1997_05 |