HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonium Chloride → 6-Methyl-1,3-dioxaindan-5-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | 5-Methyl-6-nitro-1,3-benzodioxole | HCID 4550461 | — |
| Katalysator | Iron | HCID 23925 | — |
| Lösungsmittel | Methanol--water (1/1) | HCID 22242641 | — |
| Produkt | 6-Methyl-1,3-dioxaindan-5-amine | HCID 12445340 | 94,5% |
Reaktionsschritte
A mixture of 5-methyl-6-nitro-benzo(1,3)dioxole (50 mg, 0.28 mmol), Fe (54 mg, 3.5 eq) and ammonium chloride (51.2 mg, 3.5 eq) in a 1:1 mixture of MeOH/H2O (2.8 mL) was subjected to microwave irradiation (60W, P=100 p.s.i.) at 80° C. for four 10 min periods. The brown solution was allowed to cool to r.t. and more Fe (3.5 eq) and ammonium chloride (3.5 eq) were added. The mixture was subjected to microwave irradiation (60W, P=100 p.s.i.) at 80° C. for an additional 10 min. Fe was filtered off and the solvent evaporated. The crude product was purified on an SCX cartridge (cHex/EtOAc 9:1) to give the title compound as a brown solid (40 mg, 93%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07427630B2 |
| Quelldatensatz | uspto-grants-2008_09 |
| ORD ID | ord-dc47ee82b9a8400b886e1229bfe8af8c |
| Quellennotiz | uspto-grants-2008_09 |