HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2-N-methyl-6-fluoro-1-isoquinolinone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 6-Fluoroisoquinolin-1(2H)-one | HCID 45090802 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 2-N-methyl-6-fluoro-1-isoquinolinone | HCID 69399976 | 107,5% |
Reaktionsschritte
Sodium hydride (60% in mineral oil) (211 mg, 5.27 mmol) was added to 6-fluoro-1,2-dihydroisoquinolin-1-one (716 mg, 4.39 mmol) in anhydrous DMF (6 mL) cooled in an ice bath. The mixture was stirred for about 30 min at room temperature and methyl iodide (0.328 mL, 5.27 mmol) was added dropwise. After 1 h, the reaction was judged to be about 60% complete and additional methyl iodide (0.2 mL, 3.2 mmol) was added. After about 1 h, ice and water and ethyl acetate were added to the mixture. After extractive work up with ethyl acetate, the title compound (836 mg) was obtained as a cream solid and carried on without purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09034900B2 |
| Quelldatensatz | uspto-grants-2015_05 |
| ORD ID | ord-0e5454cf6fb4431a84ed25aa1fe6640b |
| Quellennotiz | uspto-grants-2015_05 |