Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Cyanamide | HCID 9864 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 3-Benzyloxyaniline | HCID 92892 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | HCID 178419031 | HCID 178419031 | 98,4% |
Reaktionsschritte
To a suspension of 3-benzyloxyphenylamine (20.0 g, 100.35 mmol) in 1,4-dioxane (150 mL) was added cyanamide (7.39 g, 175.95 mmol followed by 4M HCl in 1,4-dioxane (44 ml, 176.00 mmol). The resulting suspension was heated at 80° C. overnight then cooled to ambient temperature and 6N NaOH (35 ml, 210.00 mmol) was added. The volume of solution was reduced to 50 ml in vacuo and the resulting precipitate was collected by filtration. The solid product was dried under vacuum overnight to afford 23.8 g in 98.4% yield. 1H NMR (MeOH-d4) δ 6.4–7.5 (m, 9H), 5.1 (s, 2H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US07084159B2 |
|---|
| Quelldatensatz | uspto-grants-2006_08 |
|---|
| ORD ID | ord-e6b1f13036c244b682cb1d3247b19d66 |
|---|
| Quellennotiz | uspto-grants-2006_08 |
|---|