関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetate | HCID 175 | — |
| 反応物 | 3-Aminopyridine | HCID 10009 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Chloro-4-(4-pyridinylmethyl)phthalazine | HCID 1944609 | — |
| 生成物 | 1-(3-Pyridylamino)-4-(4-pyridylmethyl)phthalazine | HCID 22742008 | — |
反応手順
A mixture of 0.511 g (2 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.565 g (6 mmol) 3-aminopyridine is heated for 3 h at 90° C. The residue is then distributed between acetate and 20% aqueous potassium carbonate solution. The organic phase dried over anhydrous sodium sulfate is evaporated and the residue purified on silica gel by flash chromatography using acetate/methanol mixtures (49:1 to 4:1). Title compound is obtained after crystallization of the product-containing fractions from acetonitrile and drying under HV (6 h, 80° C.); m.p. 137-139° C.; ESI-MS: (M+H)+=314.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06710047B2 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-f462d2582a3e4670a175fc0c7446c18b |
|---|
| 出典メモ | uspto-grants-2004_03 |
|---|