HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,3-Dichloroacetone → 4-(Chloromethyl)-2-(thiophen-2-yl)-1,3-oxazole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,3-Dichloroacetone | HCID 10793 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 2-Thiophenecarboxamide | HCID 22063 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 4-(Chloromethyl)-2-(thiophen-2-yl)-1,3-oxazole | HCID 2529531 | 57% |
Reaktionsbedingungen
| Temperatur | 120 °C |
|---|
Reaktionsschritte
A mixture of 2-thiophenecarboxamide (5.09 g) and 1,3-dichloroacetone (457 g) was stirred at 120° C. for 2 hours. The reaction mixture was poured into water, nautralized with potassium carbonate, and then extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4), and concentrated under reduced pressure. The residue was subjected to a silica gel column chromatography. From the fraction eluted with diethyl ether-hexane (1:9, v/v), 4-chloromethyl-2-(2-thienyl)oxazole (4.09 g, 57%) was obtained. Recrystallization from isopropylether gave colorless needles, mp 59-59° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06211215B1 |
| Quelldatensatz | uspto-grants-2001_04 |
| ORD ID | ord-c0f2cf7c7df84db1a690d728e4081640 |
| Quellennotiz | uspto-grants-2001_04 |