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Dimethylformamide → N-(4-Chlorophenyl)-4-[(pyridin-4-yl)methoxy]phthalazin-1-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 4-Hydroxymethylpyridine | HCID 11472 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-Chloro-4-(4-chloroanilino)phthalazine hydrochloride | HCID 22397278 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-(4-Chlorophenyl)-4-[(pyridin-4-yl)methoxy]phthalazin-1-amine | HCID 22397275 | — |
反応手順
A mixture of 1 g (9.16 mmol) 4-hydroxymethylpyridine, 0.44 g (11.0 mmol) sodium hydride (60% dispersion in oil) and 15 ml DMF is incubated for 20 min at 0° C. while stirring in a nitrogen atmosphere. At RT, 1 g (3.07 mmol) 1-chloro-4-(4-chloroanilino)phthalazine hydrochloride is added to the mixture, which is stirred for about 1 h at 500C and for 15 h at 80° C. Addition to the reaction mixture of a little water, evaporation under vacuum, recrystallization of the residue from methanol, and drying under HV yield the title compound with a water content of 3.36%; m.p. 139-141° C.; ESI-MS: (M+H)+=363.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06514974B2 |
| 出典データセット | uspto-grants-2003_02 |
| ORD ID | ord-190c9a9b888647919afaa2bd6bd7b723 |
| 出典メモ | uspto-grants-2003_02 |