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Triethylamine → 2'-Chloro-5'-(cyclohexanecarbonyl-amino)-biphenyl-4-carboxylic acid [4-(4-methyl-piperazin-1-ylmethyl)-phenyl]-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| 反応物 | 4-((4-Methylpiperazin-1-yl)methyl)aniline | HCID 3153996 | — |
| 反応物 | 2'-Chloro-5'-(cyclohexanecarbonyl-amino)-biphenyl-4-carboxylic acid | HCID 59822346 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2'-Chloro-5'-(cyclohexanecarbonyl-amino)-biphenyl-4-carboxylic acid [4-(4-methyl-piperazin-1-ylmethyl)-phenyl]-amide | HCID 67371224 | 32.6% |
反応手順
A mixture of 2′-Chloro-5′-(cyclohexanecarbonyl-amino)-biphenyl-4-carboxylic acid (103 mg), 4-(4-methyl-piperazin-1-ylmethyl)-phenylamine (59 mg) and HBTU (148 mg) in dry DMF (10 ml) containing triethylamine (362 μl) was stirred at room temp for 18 h. Most of the DMF was evaporated and the residue diluted with water. The resulting solid was collected by filtration. This material was then purified by reverse phase Prep HPLC giving the title compound as a yellow solid (51 mg)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08008303B2 |
| 出典データセット | uspto-grants-2011_08 |
| ORD ID | ord-f65289ecdf12435ebe8487ff42e309ac |
| 出典メモ | uspto-grants-2011_08 |