HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2-Amino-3-(2-chloro-4,5-methylenedioxybenzyloxy)-pyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 2-Amino-3-Hydroxypyridine | HCID 28114 | — |
| Edukt | 6-Chloropiperonyl chloride | HCID 90113 | — |
| Katalysator | Trioctylmethylammonium chloride | HCID 21218 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | Sodium Hydroxide | HCID 14798 | — |
| Produkt | 2-Amino-3-(2-chloro-4,5-methylenedioxybenzyloxy)-pyridine | HCID 20077049 | 24,3% |
Reaktionsschritte
To a solution of 2-amino-3-hydroxypyridine (9.75 g, 0.0886 mol) in dichloromethane (55 ml) and 40% sodium hydroxide (55 ml) was added Adogen 464 (5 ml) and 6-chloropiperonyl chloride (20 g, 0,0975 mol) with vigorous stirring. The mixture was stirred at room temperature for 16 hours. Water (55 ml) was added and the mixture extracted with dichloromethane. The combined organic layers were dried and evaporated, and the residue purified by flash chromatography (silica, 1% methanol/dichloromethane) and trituration with ether to yield the title compound (6 g), m.p. 100°-104° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05409943 |
| Quelldatensatz | uspto-grants-1995_04 |
| ORD ID | ord-c18b5067f4074f708abea2967a7af022 |
| Quellennotiz | uspto-grants-1995_04 |