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 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 3-Chloropyridine-2-carboxylic acid | HCID 824632 | — |
| 反応物 | 4-Iodo-N1-methylbenzene-1,2-diamine | HCID 66064280 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 71247910 | HCID 71247910 | 73.4% |
反応手順
A mixture of 4-iodo-N1-methyl-benzene-1,2-diamine (850 mg), 3-chloro-pyridin-2-carboxylic acid (590 mg), WSC (790 mg), HOBt (46 mg), and pyridine (10 ml) was stirred at 100° C. for 12 hours. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 2-(3-chloro-pyridin-2-yl)-5-iodo-1-methyl-1H-benzimidazole (930 mg), which is hereinafter referred to as “intermediate compound (M6-21)”.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09353110B2 |
|---|
| 出典データセット | uspto-grants-2016_05 |
|---|
| ORD ID | ord-c8ba6e03cd7f44a28e1ac82f19806503 |
|---|
| 出典メモ | uspto-grants-2016_05 |
|---|
