HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 6-methyl-1H-indazol-5-ol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Lithium Hydroxide | HCID 3939 | — |
| Edukt | Potassium bisulfate | HCID 516920 | — |
| Edukt | 1-acetyl-6-methyl-1H-indazol-5-yl acetate | HCID 69430758 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 6-methyl-1H-indazol-5-ol | HCID 22934018 | 92% |
Reaktionsschritte
A 2M-aqueous lithium hydroxide solution (1.46 ml, 2.93 mmol) was added dropwise to a solution of 1-acetyl-6-methyl-1H-indazol-5-yl acetate (340 mg, 1.46 mmol) in a mixture of methanol (2.0 ml) and tetrahydrofuran (1.0 ml) at room temperature. After 1 hour, the reaction mixture was adjusted to pH 4 with a 0.5M-aqueous potassium hydrogensulfate solution. The resulting solution was poured into water (50 ml) and extracted with ethyl acetate (30 ml×3), and the extract solution was dried over anhydrous magnesium sulfate. The extract solution dried was concentrated under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) to obtain 6-methyl-1H-indazol-5-ol (199 mg, 92%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07199147B2 |
| Quelldatensatz | uspto-grants-2007_04 |
| ORD ID | ord-3700daeff9204b4b9156fef467cf8cb0 |
| Quellennotiz | uspto-grants-2007_04 |