HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2-(5-Chlorothiophen-2-yl)-2-oxoacetic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Ethyl 5-chlorothiophene-2-glyoxylate | HCID 14452581 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 2-(5-Chlorothiophen-2-yl)-2-oxoacetic acid | HCID 13807692 | — |
Reaktionsschritte
(5-Chlorothiophen-2-yl)-oxo-acetic acid ethyl ester (8.62 g, 39.4 mmol) was dissolved in a mixture of 100 ml water and 100 ml methanol, then treated with 10 N NaOH (5.9 ml, 59 mmol) at room temperature for 20 hours. The reaction was then poured into 200 ml 3N HCl, and extracted with ethyl acetate (2×100 ml). The combined ethyl acetate extracts were dried over Na2SO4 and concentrated under vacuum to provide Preparation 1b (6.89 g, 92%). The product was then recrystallized from hexane/ether. MS (M−H)−: 189.10; 1H NMR (300 MHz, CDCl3) δ9.07 (1H, br s), 8.32 (1H, d, J=4.2 Hz), 7.10 (1H, d, J=4.2 Hz). IR (KBr) 3270, 3099, 1765, 1744, 1675, 1514, 1411, 1325 cm−1.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06613786B2 |
| Quelldatensatz | uspto-grants-2003_09 |
| ORD ID | ord-4c69e217b275422aa89990743e43e26b |
| Quellennotiz | uspto-grants-2003_09 |