HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 6-Bromo-2-methoxypyridin-3-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | N-bromobutanimide | HCID 67184 | — |
| Edukt | 3-Amino-2-methoxypyridine | HCID 2737488 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 6-Bromo-2-methoxypyridin-3-amine | HCID 10536137 | 80,5% |
Reaktionsschritte
A solution of 2-methoxypyridin-3-amine (39.4 g) in N,N-dimethylformamide (200 mL) was cooled to −30° C., and a solution of N-bromosuccinimide (62.1 g) in N,N-dimethylformamide (100 mL) was added dropwise. After stirring for 30 minutes, the reaction solution was poured into water and extracted with chloroform. The organic layer was sequentially washed with a saturated sodium sulfite solution, water and brine and dried over sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1→4:1) to give 6-bromo-2-methoxypyridin-3-amine as a yellow powder (51.9 g, 80%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08822503B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-1f69f2bc68bc4c5eb7d97fee0c8c7ec9 |
| Quellennotiz | uspto-grants-2014_09 |