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1-Hydroxybenzotriazole → 3-ethylsulfanyl-N-(5-pentafluoroethylpyridin-2-yl)picolinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 5-(Perfluoroethyl)pyridin-2-amine | HCID 49853555 | — |
| 反応物 | 3-(Ethylsulfanyl)pyridine-2-carboxylic acid | HCID 79006954 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 3-ethylsulfanyl-N-(5-pentafluoroethylpyridin-2-yl)picolinamide | HCID 118205940 | 29.4% |
反応手順
A mixture of 0.63 g of 2-amino-5-pentafluoroethylpyridine, 0.55 g of 3-ethylsulfanylpicolinic acid, 1.0 g of EDCI hydrochloride, 0.04 g of HOBt and 5 mL of pyridine was stirred at room temperature overnight. A saturated aqueous sodium bicarbonate solution was poured to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure, and the resulting residue was applied to a silica gel column chromatography to obtain 0.33 g of 3-ethylsulfanyl-N-(5-pentafluoroethylpyridin-2-yl)picolinamide (hereinafter, referred to as Compound of Present Invention 46).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09185910B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-2d266a5a559a4c53905211a28e46641b |
| 出典メモ | uspto-grants-2015_11 |