関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Chloro-4-(4-pyridinylmethyl)phthalazine | HCID 1944609 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Benzylamino-4-(4-pyridylmethyl)phthalazine | HCID 9927362 | — |
反応手順
A mixture of 1.28 g (5 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 1.64 ml (15 mmol) benzylamine is stirred for 4 min at 90° C. under a nitrogen atmosphere. The reaction mixture is then distributed between dichloromethane 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 and acetate/methanol (20:1). Title compound is obtained after crystallization of the product-containing fractions from acetonitrile and drying under HV (8 h, 80° C.); m.p. 137-138° C.; ESI-MS: (M+H)+=327.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06710047B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-41ddeae85a6846059185028bc1fd748f |
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| 出典メモ | uspto-grants-2004_03 |
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