HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → 5,6,7,8-tetrahydro-4H-cyclohepta[b]thiophen-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | 5-(2-Thienyl)valeric acid | HCID 152324 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 5,6,7,8-tetrahydro-4H-cyclohepta[b]thiophen-4-one | HCID 12341557 | 34.5% |
Reaction Steps
To a mixture of 5-(2-thienyl)pentanoic acid (5.04 g) and toluene (50 ml) was dropwise added trifluoroacetic anhydride (6.95 ml) over 1 minute with ice-water cooling. The reaction mixture was stirred at room temperature (r.t.) overnight, and was poured into a mixture of a saturated aqueous solution of sodium hydrogen carbonate (NaHCO3) and AcOEt. The organic layer was washed with water and brine, and dried over MgSO4, and evaporated. The resulting oil was purified by chromatography on silica gel (SiO2) (20% AcOEt in n-hexane as eluent). The fractions including the object compound were combined and evaporated to give 4-oxo-5,6,7,8-tetrahydro-4H-cyclohepta[b]thiophene (1.57 g) as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06274619B1 |
| Source dataset | uspto-grants-2001_08 |
| ORD ID | ord-276b32f8e198470cbe1944636cea0afa |
| Source note | uspto-grants-2001_08 |