HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Chloroacetyl chloride → 1-(5-Acetyl-thiophen-2-yl)-2-chloro-ethanone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Chloroacetyl chloride | HCID 6577 | — |
| Edukt | 2-Acetylthiophene | HCID 6920 | — |
| Edukt | Chloromethyl Thienyl Ketone deriv. 5 | HCID 6539169 | — |
| Produkt | 1-(5-Acetyl-thiophen-2-yl)-2-chloro-ethanone | HCID 4165708 | 25% |
Reaktionsschritte
General procedure described for compounds 1 and 2 starting from 2-acetylthiophene and chloroacetyl chloride. Purified by column chromatography column (hexane:ethyl acetate 3:1), yield 25%, m.p.: 94-95° C., 1H-NMR (CDCl3): δ8.3 (d, J=4.2 Hz, 1H, Ar), 8.1 (d, J=4.2 Hz, 1H, Ar), 4.55 (s, 2H, CH2), 2.6 (s, 3H, CH3); 13C-NMR (CDCl3). δ193.0 (CO), 187.8 (CO), 148.3 (C—CO), 142.0 (CH), 141.7 (C—CO), 133.7 (CH), 48.3 (CH2), 29.2 (CH3); M/z (EI): 204, 202 (M +, 4, 10%), 153 (M-CH2Cl, 100%); HPLC: Column μ Bondapack C18, 5 μm, 300 A, (300×3.9 mm), Purity 98%, r.t.=3.50 min, acetonitrile/H2O (0.05% H3PO4+0.04% Et3N) 50/50.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06747057B2 |
| Quelldatensatz | uspto-grants-2004_06 |
| ORD ID | ord-1ebba97bc0534d7e81d9088cc6554563 |
| Quellennotiz | uspto-grants-2004_06 |