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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → N'-[4-(Benzyloxy)phenyl]-2-chloropyridine-3-carbohydrazide
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 | 2-Chloronicotinic acid | HCID 76258 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-Benzyloxyphenylhydrazine | HCID 561392 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N'-[4-(Benzyloxy)phenyl]-2-chloropyridine-3-carbohydrazide | HCID 86704974 | 67.5% |
反応手順
To a solution of 2-chloropyridine-3-carboxylic acid (3.30 g) in DMF (50 ml) were added [4-(benzyloxy)phenyl]hydrazine (5.0 g), HOBt (3.7 g), EDCI (4.6 g) and diisopropylethylamine (9.0 g), and the mixture was stirred at room temperature for 12 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layers were combined, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (5.0 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09029388B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-bfd42e8e04b5403f81fb3b812034444f |
| 出典メモ | uspto-grants-2015_05 |