HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrogen Peroxide → 4,4-Diethyl-4,5-dihydro-3H-pyrazole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrogen Peroxide | HCID 784 | — |
| Edukt | 1,3-Diamino-2,2-diethylpropane | HCID 432589 | — |
| Edukt | Sodium Hypochlorite | HCID 23665760 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 4,4-Diethyl-4,5-dihydro-3H-pyrazole | HCID 21823534 | 77% |
Reaktionsschritte
2,2-Diethyl-propane-1,3-diamine (5.0 g) was taken up in a mixture of H2O (40 mL) and MeOH (10 mL), and cooled in an ice bath. Simultaneously, H2O2 (24.2 mL of a 30% solution, 6 equiv.) and NaClO (54.9 mL of a 10% solution, 2.4 equiv.) were added dropwise, the ice bath was removed, and the mixture was stirred for 2 h. at room temperature. Extraction with DCM, drying over Na2SO4 and evaporation under reduced pressure yielded 3.51 g of a clear, yellow liquid containing 77% of the anticipated product and 23% of the diamine starting material. This material was used in subsequent steps without further purification. 1H NMR (400 MHz, CDCl3) δ 0.78 (t, J=7.5 Hz, 6H), 1.36 (q, J=7.5 Hz, 4H), 4.14 (s, 4H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08722887B2 |
| Quelldatensatz | uspto-grants-2014_05 |
| ORD ID | ord-a9d77dddad274685bd831afc3efc3579 |
| Quellennotiz | uspto-grants-2014_05 |