HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Benzoyl Peroxide → 3-Methoxy-2-nitro-6-pyridylmethyl bromide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Benzoyl Peroxide | HCID 7187 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | N-bromobutanimide | HCID 67184 | — |
| Edukt | 3-Methoxy-6-methyl-2-nitropyridine | HCID 2727965 | — |
| Lösungsmittel | Carbon Tetrachloride | HCID 5943 | — |
| Produkt | 3-Methoxy-2-nitro-6-pyridylmethyl bromide | HCID 14405124 | — |
Reaktionsschritte
A mixture of 3-methoxy-6-methyl-2-nitropyridine (10.08 g, 60 mmol), NBS (9.79 g, 55 mmol), and benzoyl peroxide (2 g, 6 mmol) in CCl4 (250 mL) was refluxed for 56 hours under nitrogen atmosphere. The reaction mixture was added 100 mL 1M NaOH aq. and extracted using ethyl acetate (3×300 mL). The combined organic layer was dried over Mg2SO4 and filtered. The solvent was evaporated to yield a brown oily. 1H-NMR (CDCl3): δ 3.99 (s, 3H, OCH3), 4.51 (s, 2H, CH2), 7.55 (d, 1H, J=8.8 Hz, Py-H), 7.70 (d, 1H, J=8.4 Hz, Py-H). HR-MS (ESI+) m/z 246.9600 [M+1]+ C7H7BrN2O3 requires 245.9640.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08829003B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-836af7366fa74fcda1241520e5f003c4 |
| Quellennotiz | uspto-grants-2014_09 |