Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Carbon Disulfide | HCID 6348 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | 1-Benzofuran-5-carbohydrazide | HCID 68664129 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | HCID 178527940 | HCID 178527940 | 36% |
Reaktionsschritte
To a solution of 1-benzofuran-5-carbohydrazide (1.50 g, 8.51 mmol) in ethanol (60 mL) were added potassium hydroxide (0.72 g, 12.8 mmol) and carbon disulfide (15.3 mL, 25.5 mmol), and the resulting mixture was stirred at room temperature for 5 hr. The reaction mixture was concentrated under reduced pressure, a mixture of the residue and N,N-dimethylformamide (30 mL) was tightly sealed in a vial, and the microwave was irradiated at 150° C. for 1 min. After cooling, the reaction mixture was acidified with 1M hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from hexane/ethyl acetate to give the title compound (0.66 g, yield 36%) as colorless crystals.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08492378B2 |
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| Quelldatensatz | uspto-grants-2013_07 |
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| ORD ID | ord-b92e4429247045c6bb8017f35dc52523 |
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| Quellennotiz | uspto-grants-2013_07 |
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