HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrogen Peroxide → HCID 59339474, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrogen Peroxide | HCID 784 | — |
| Edukt | [4-(Aminomethyl)oxan-4-yl]methanamine | HCID 68738 | — |
| Edukt | Sodium Hypochlorite | HCID 23665760 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 59339474 | HCID 59339474 | 85% |
Reaktionsschritte
C-(4-Aminomethyl-tetrahydro-pyran-4-yl)-methylamine (1.0 g) was taken up in a mixture of H2O (10 mL) and MeOH (2.5 mL), and cooled in an ice bath. Simultaneously, H2O2 (4.8 mL of a 30% solution, 6 equiv.) and NaClO (12.4 mL of a 10% solution, 2.4 equiv.) were added dropwise, the ice bath was removed, and the mixture was stirred overnight at room temperature. Extraction with DCM, drying over Na2SO4 and evaporation under reduced pressure yielded 380 mg of a clear, light-yellow liquid containing 85% of the anticipated product and 15% of the diamine starting material. This material was used in subsequent steps without further purification. 1H NMR (400 MHz, CDCl3) δ 1.49 (t, 4H), 3.65 (t, 4H), 4.28 (s, 4H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07728018B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-f33760f47a354d128b5ea74e5ca6a297 |
| Quellennotiz | uspto-grants-2010_06 |