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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 58116841、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Piperazin-1-yl-pyrrolidin-1-yl-methanone | HCID 2760443 | — |
| 反応物 | 4-Bromocrotonic acid | HCID 6436411 | — |
| 反応物 | (3,4-Dichloro-phenyl)-(5,6,7,8-tetrahydro-9-thia-1,3,7-triaza-fluoren-4-yl)-amine | HCID 58116912 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 58116841 | HCID 58116841 | 10% |
反応手順
(2E)-4-Bromobut-2-enoic acid (106 mg, 0.64 mmol) and piperazin-1-yl(pyrrolidin-1-yl)methanone (125 mg, 0.68 mmol) were dissolved in DCM (5.0 mL), and DIPEA (111 mg, 0.85 mmol) was added. The mixture was stirred at rt for 2 h. Subsequently, the compound from Example 15A (150 mg, 0.43 mmol), DIPEA (55 mg, 0.43 mmol) and EDCI (82 mg, 0.43 mmol) were added. The reaction was stirred at 50° C. overnight. Then, water was added, and the mixture was extracted three times with DCM. The combined organic layers were dried over sodium sulfate. The solvent was removed in vacuo, and the residue was purified by preparative HPLC to yield 25 mg (10%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524722B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-907f815ae1db4702b9a88f10da798df7 |
| 出典メモ | uspto-grants-2013_09 |