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Sodium Carbonate → 1-Benzyl-4-((R)-3-methyl-piperazin-1-yl)-phthalazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1-Benzyl-4-chlorophthalazine | HCID 6404566 | — |
| 反応物 | 2-Methylpiperazine, (R)- | HCID 7330434 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-Benzyl-4-((R)-3-methyl-piperazin-1-yl)-phthalazine | HCID 44186248 | 58% |
反応手順
Solid Na2CO3 (200 mg, 1.9 mmol, 1.9 eq) is added to a solution of 1-benzyl-4-chlorophthalazine (250 mg, 0.98 mmol, 1 eq) and (R)-2-methyl-piperazine (400 mg, 4.0 mmol, 4.0 eq) in dioxane (5 mL) in a microwave vial. The vial is sealed and irradiated in the microwave at 150° C. (high absorption setting) for 30 minutes. The reaction mixture is filtered and concentrated, then diluted with EtOAc (50 mL) and water (15 mL). The organic fraction washed with water and then brine, then is dried over sodium sulfate. The solvent is evaporated under reduced pressure to afford the title compound as a white solid (180 mg, 58% yield).
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-254f7c629db147839715ceb1129a9f43 |
| 出典メモ | uspto-grants-2013_09 |