HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrogen Peroxide → 2,3-Diaza-spiro[4.5]dec-2-ene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrogen Peroxide | HCID 784 | — |
| Edukt | [1-(Aminomethyl)cyclohexyl]methanamine | HCID 71994 | — |
| Edukt | Sodium Hypochlorite | HCID 23665760 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 2,3-Diaza-spiro[4.5]dec-2-ene | HCID 59339453 | — |
Reaktionsschritte
C-(1-Aminomethyl-cyclohexyl)-methylamine (10.0 g) was taken up in a mixture of H2O (40 mL) and MeOH (10 mL), and cooled in an ice bath. Simultaneously, H2O2 (44.3 mL of a 30% solution, 6 equiv.) and NaClO (125.5 mL of a 10% solution, 2.4 equiv.) were added dropwise, the ice bath was removed, and the mixture was stirred for 45 min. at room temperature. Extraction with DCM, drying over Na2SO4 and evaporation under reduced pressure, yielded 8.7 g of a clear, light-yellow liquid. 1H NMR (400 MHz, CDCl3) δ 1.24-1.53 (m, 10H), 4.17 (s, 4H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07728018B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-2504d08685a64c35a6ba654bf4472cd6 |
| Quellennotiz | uspto-grants-2010_06 |