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Water → 2-Amino-3-(2-chloro-4,5-methylenedioxybenzyloxy)-pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Amino-3-Hydroxypyridine | HCID 28114 | — |
| 反応物 | 6-Chloropiperonyl chloride | HCID 90113 | — |
| 触媒 | Trioctylmethylammonium chloride | HCID 21218 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 2-Amino-3-(2-chloro-4,5-methylenedioxybenzyloxy)-pyridine | HCID 20077049 | 24.3% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05409943 |
| 出典データセット | uspto-grants-1995_04 |
| ORD ID | ord-c18b5067f4074f708abea2967a7af022 |
| 出典メモ | uspto-grants-1995_04 |