HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-Methyl-2-butanone → 2,3,3-Trimethyl-4-carboxy-3H-indole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-Methyl-2-butanone | HCID 11251 | — |
| Edukt | 3-Hydrazinobenzoic acid | HCID 2736521 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Sulfuric Acid | HCID 1118 | — |
| Produkt | 2,3,3-Trimethyl-4-carboxy-3H-indole | HCID 66597718 | 81,4% |
Reaktionsschritte
A solution of 3-hydrazinobenzoic acid (30.0 g, 197 mmol), isopropylmethylketone (31.7 mL, 296 mmol) in ethanol (500 mL) and sulfuric acid (5 mL) was heated under reflux in an oil bath for 20 h. After cooling to ambient temperature the solvent was evaporated off under reduced pressure to a small volume of ˜200 mL. Collected the solid with a filter funnel, washed with iPrOH (3×30 mL) and ethyl ether (3×30 mL) and dried. Further drying of the solid in an oven at 45° C. under high vacuum for 18 h provided 32.59 g (81.3%) of the product. (This is [0148]1.2)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09441270B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-284a73482a9b4cd98a41cec19e8ad20d |
| Quellennotiz | uspto-grants-2016_09 |