HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Hydroxide → 2-Benzyl-1-bromo-6-methoxypyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | Bromine | HCID 24408 | — |
| Edukt | Sodium Sulfite | HCID 24437 | — |
| Edukt | Potassium Bromide | HCID 253877 | — |
| Edukt | 2-Benzyl-6-methoxypyridine | HCID 21942274 | — |
| Katalysator | HCID 22266888 | HCID 22266888 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 2-Benzyl-1-bromo-6-methoxypyridine | HCID 18182294 | — |
Reaktionsschritte
A mixed solution of 17 ml of bromine, 90 g of potassium bromide and 450 ml of water was added dropwise into a mixture of 60 g of 2-benzyl-6-methoxypyridine (Production Example 2-b), 90 g of potassium bromide, 450 ml of water, 20 g of potassium hydroxide and 2.5 g of tetraammonium chloride over 2 hours under stirring in an ice bath. After stirring overnight as it was, sodium sulfite was added thereto and the mixture was extracted with hexane. The organic phase was washed with water and brine, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was subjected to silica gel column chromatography to elute with 0.5-1.5% of ethyl acetate/hexane, to give 72.5 g of the target compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06599917B1 |
| Quelldatensatz | uspto-grants-2003_07 |
| ORD ID | ord-0314bc1e8d6b4fe0a3167db30808daec |
| Quellennotiz | uspto-grants-2003_07 |