HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2-Methylthiophene-3-carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Ethyl 2-methylthiophene-3-carboxylate | HCID 10464736 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 2-Methylthiophene-3-carboxylic acid | HCID 4625409 | 77% |
Reaktionsschritte
Ethyl 2-methyl-3-thiophenecarboxylate (3.42 g, 20.09 mmol; see step (ii) above) was dissolved in ethanol (5 mL) to which was added a solution of sodium hydroxide (3.2145 mg, 80.362 mmol) in water (10 mL). The reaction mixture was heated under reflux for 2 h. The volume was reduced to half under reduced pressure at 40° C. and the residue was cooled with ice water. Dilute HCl was added dropwise with stirring until pH 2. The white solid material was filtered off, washed with water and dried under reduced pressure at 50° C. to give the required material (2.1850 mg, 77% yield), m.p. 115-117° C., lit. m.p. 116-117° C. (see D. W. Knight, A. P. Nott J. Chem. Soc., Perkin Trans. 1 791-794 (1983)).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07700765B2 |
| Quelldatensatz | uspto-grants-2010_04 |
| ORD ID | ord-f49607a9e93249daaab070e2dcce2746 |
| Quellennotiz | uspto-grants-2010_04 |