HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sulfamide → N-(2-cyano-3-methylphenyl)sulfamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sulfamide | HCID 82267 | — |
| Edukt | 2-Amino-6-methylbenzonitrile | HCID 279973 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | N-(2-cyano-3-methylphenyl)sulfamide | HCID 67097231 | — |
Reaktionsschritte
A solution of 2-amino-6-methylbenzonitrile (1.32 g, 10 mmol) and sulfamide (4.81 g, 50 mmol) in dry 1,4-dioxane (50 mL) was refluxed under nitrogen for 3 days. After the reaction mixture was cooled down to room temperature, the precipitate was filtered and washed with dioxane. The filtrate was concentrated under reduced pressure, and the residue was purified by chromatography on silica gel eluting with EtOAc/hexanes (3:7) to give the title compound as a pale-white solid. 1H NMR (400 MHz, DMSO-d6) δ2.44 (s, 3H), 7.19-7.21 (m, 3H), 7.39-7.41 (d, J=8.4 Hz, 1H), 7.53 (t, J=8.0 Hz, 1H), 9.41 (s, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08541421B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-35795869fc134710aa3df281aef8b985 |
| Quellennotiz | uspto-grants-2013_09 |