HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tetrahydrofuran → 3-[4-chloro-2-fluoro-5-(2-nitrophenoxy)phenyl]-2-[(1-cyclopentylidene)aminooxy]-6-trifluoromethyl-4(3H)-pyrimidinone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Cyclopentanone, oxime | HCID 14500 | — |
| Edukt | 2-chloro-3-[4-chloro-2-fluoro-5-(2-nitrophenoxy)phenyl]-6-trifluoromethyl-4(3H)-pyrimidinone | HCID 10238633 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 3-[4-chloro-2-fluoro-5-(2-nitrophenoxy)phenyl]-2-[(1-cyclopentylidene)aminooxy]-6-trifluoromethyl-4(3H)-pyrimidinone | HCID 22660238 | 84,7% |
Reaktionsschritte
A mixture of 2-chloro-3-[4-chloro-2-fluoro-5-(2-nitrophenoxy)phenyl]-6-trifluoromethyl-4(3H)-pyrimidinone(1.28 g, 0.0027 mol), cyclopentanone oxime(027 g, 0.0027 mol), potassium carbonate(0.38 g, 0.027 mol) and tetrahydrofuran(11 ml) was heated under reflux for 3 hours. The reaction mixture was poured into water, extracted with ethyl acetate, and washed with brine. The organic phase was dried over anhydrous sodium sulfate, and concentrated. The residue was purified by column chromatography on silica gel(20% ethyl acetate/hexane) to give compound II-3 (1.23 g, yield 84.7%) as a white amorphous solid, m.p.76-78° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06806367B2 |
| Quelldatensatz | uspto-grants-2004_10 |
| ORD ID | ord-bd04dc98f49b41f38d2df63e165da3de |
| Quellennotiz | uspto-grants-2004_10 |