HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Iodine → 3,5-diethyl 4-iodo-1H-pyrazole-3,5-dicarboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Iodine | HCID 807 | — |
| Edukt | Sodium Thiosulfate | HCID 24477 | — |
| Edukt | diethyl 1H-pyrazole-3,5-dicarboxylate | HCID 142184 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 3,5-diethyl 4-iodo-1H-pyrazole-3,5-dicarboxylate | HCID 11739230 | — |
Reaktionsschritte
To a solution of 10 g 1H-Pyrazole-3,5-dicarboxylic acid diethyl ester in 400 ml acetonitrile 13 g ammonium cerium(iv) nitrate (CAN) and 7.17 g iodine were added and the mixture was heated to reflux for 5 h. Then, after cooling to RT, 30 ml sat. sodium thiosulfate solution were added. The mixture was extracted with ethyl acetate (3×100 ml), the combined organic layers were washed with water and then dried over MgSO4, filtered and the solvents were removed under reduced pressure. The residue was filtered through a pad of silica gel eluting with heptane/ethyl acetate 1:1.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07429581B2 |
| Quelldatensatz | uspto-grants-2008_09 |
| ORD ID | ord-0d5a393a7b0d42febfff4291922d7261 |
| Quellennotiz | uspto-grants-2008_09 |