HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Acid → Methyl alpha-Methyl-1-nitro-1,2-dihydro-6-azanaphthalene-2-acetate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | Acetonitrile | HCID 6342 | — |
| Edukt | 5-Nitroisoquinoline | HCID 69085 | — |
| Edukt | Tris(dimethylamino)sulfonium difluorotrimethylsilicate | HCID 9795567 | — |
| Lösungsmittel | Hexane | HCID 8058 | — |
| Produkt | Methyl alpha-Methyl-1-nitro-1,2-dihydro-6-azanaphthalene-2-acetate | HCID 13507926 | — |
Reaktionsschritte
A flame dried 50 mL flask fitted with an addition funnel was charged with 0.872 g (500 mmol) of 5-nitroisoquinoline and 0.95 mL (5.1 mmol) of MTS. An acetonitrile solution of 1.40 g (5.09 mmol) of TASF was slowly added to the reaction mixture in 15 min at -78° C. The mixture was stirred for 22 h at that temperature. One mL of acetic acid in 5 mL of hexane was added, and reaction was warmed to room temperature. After 30 min, 40 mL of water was added. The solid which precipitated out was collected and analyzed. The product yield was 0.972 g (74%). The product material was analyzed by infrared spectroscopy, nuclear magnetic resonance spectroscopy, and mass spectrometry.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05164499 |
| Quelldatensatz | uspto-grants-1992_11 |
| ORD ID | ord-02f61dd96e9b44fa8d5cc71fd42e8da8 |
| Quellennotiz | uspto-grants-1992_11 |