HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl 2-thiopheneglyoxylate → [(3-Methyl-butyl)-hydrazono]-thiophen-2-yl-acetic acid ethyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl 2-thiopheneglyoxylate | HCID 77693 | — |
| Edukt | (3-Methylbutyl)hydrazine | HCID 18696583 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | [(3-Methyl-butyl)-hydrazono]-thiophen-2-yl-acetic acid ethyl ester | HCID 72562995 | 47,1% |
Reaktionsbedingungen
| Temperatur | 80 °C |
|---|
Reaktionsschritte
To a solution of oxo-thiophen-2-yl-acetic acid ethyl ester (1d) (3.97 g, 21.6 mmol) in absolute ethanol (100 mL), (3-Methyl-butyl)-hydrazine (2b) (2.0 g, 19.6 mmol) was added. The mixture was stirred at 80° C. under N2 atmosphere for 2-25 hours. The reaction mixture was concentrated under reduced pressure and the residue was purified by flash chromatography on silica gel to give the desired product (3d) (2.48 g) that was directly used in the next step. LC-MS (ESI+): m/e 269.2 [M+1]+, 537.4 [2M+1]+, 559.0 [2M+Na]+ (exact ms: 268.12).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07425552B2 |
| Quelldatensatz | uspto-grants-2008_09 |
| ORD ID | ord-87f0c78e6581409aafe2d4313913c391 |
| Quellennotiz | uspto-grants-2008_09 |