化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 6-[4-(4-Chloro-phthalazin-1-yl)-piperazin-1-yl]-nicotinic acid ethyl ester
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 | Ethyl 6-(piperazin-1-yl)nicotinate | HCID 14987933 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-[4-(4-Chloro-phthalazin-1-yl)-piperazin-1-yl]-nicotinic acid ethyl ester | HCID 57471616 | 49% |
反応手順
Combine 6-piperazin-1-yl-nicotinic acid ethyl ester (1.30 g, 5.40 mmol), 1,4-dichlorophthalazine (932 mg, 4.59 mmol), triethylamine (1.78 mL, 13.50 mmol), and NMP (8 mL) and heat to 85° C. for 6 h. Cool to room temperature, dilute with H2O (50 mL) and extract organics with EtOAc (3×50 mL). Combined organic layers are dried over MgSO4 and concentrated. Resulting solid is triturated with EtOAc to give the title compound as a fine tan powder (895 mg, 49% 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-1f3c4c1675544c09b427902408c8625c |
| 出典メモ | uspto-grants-2013_09 |