関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | 1,4-Dichlorophthalazine | HCID 78490 | — |
| 反応物 | 6-(Piperazin-1-yl)pyridine-3-carbonitrile | HCID 2737184 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-[4-(4-Chloro-phthalazin-1-yl)-piperazin-1-yl]-nicotinonitrile | HCID 44186379 | 51.1% |
反応手順
To a 100-mL round-bottom flask is added 6-piperazin-1-yl-nicotinonitrile (9.60 g, 50 mmol), 1,4-dichlorophthalazine (11.2 g, 55.1 mmol, 1.1 eq), Et3N (3.5 mL, 250 mmol, 5 eq.), and NMP (100 mL). The mixture is heated to 80° C. for 2.5 h. Upon cooling to room temperature, the reaction is poured into H2O (500 mL) and the precipitate isolated by filtration, rinsing with additional H2O. Crude material is purified by recrystallization (CH2Cl2:heptanes) to afford 8.96 g title compound as a beige solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08536168B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-69b2432fdf324f2db2ebb0d08d6fe53f |
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| 出典メモ | uspto-grants-2013_09 |
|---|
