HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 9926427, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 21183833 | HCID 21183833 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 9926427 | HCID 9926427 | — |
Reaction Steps
A solution of ethyl 2,4-dioxo-4-(5-phenethylthiophen-2-yl)butanoate (125 mg, 0.378 mmol), aqueous sodium hydroxide (1.2 mL, 1M, 1.2 mmol), and THF (5 mL) in methanol (5 mL) was stirred at rt overnight. The resultant mixture was treated with aq HCl (1.3 mL. 1M), and concentrated under vacuum. The residue was partitioned between brine and dichloromethane. The organic extract was dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum to provide off-white solid. Recrystallization of the solid from a mixture dichloromethane and hexane provided the title compound. 1H NMR (CDCl3) δ 7.72 (d, J=3.1 Hz, 1H), 7.35-7.15 (m, 5H), 6.94 (s, 1H), 6.86 (d, J=3.1 Hz, 1H), 3.22 (d, J=8.1 Hz, 2H), 3.03 (d, J=8.1 Hz, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06262055B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-a82962135cc443eda53e5fa1b16d039c |
| Source note | uspto-grants-2001_07 |