関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Aminopyridine | HCID 10009 | — |
| 反応物 | Pivaloyl chloride | HCID 62493 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,2-dimethyl-N-(pyridin-3-yl)propanamide | HCID 4655044 | 75% |
反応手順
To an ice-cooled solution of 3-aminopyridine (6 g, 63.8 mmol) and triethylamine (9.72 mL, 70.2 mmol) in 124 mL of dichloromethane under argon, was carefully added pivaloyl chloride (7.92 mL, 64.4 mmol) in 16 mL of dichloromethane. After the addition was completed, the reaction mixture was stirred at 0° C. for 15 minutes and at room temperature for 18 hours. The mixture was washed with water, aqueous 4% sodium bicarbonate, brine, dried over sodium sulphate and the solvent removed under reduced pressure. The residue was purified by column chromatography on silica flash, using hexane/ethyl acetate (85:15) as eluents, to yield the title compound (8.5 g, 75%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07906530B2 |
|---|
| 出典データセット | uspto-grants-2011_03 |
|---|
| ORD ID | ord-f27acf8f24c948bdabc50eece916231a |
|---|
| 出典メモ | uspto-grants-2011_03 |
|---|