反応式
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.C(N(CC)CC)C.[C:15](Cl)(=[O:20])[C:16]([CH3:19])([CH3:18])[CH3:17]>ClCCl>[CH3:17][C:16]([CH3:19])([CH3:18])[C:15]([NH:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1)=[O:20]参加物
5
反応条件
- 温度
- 0 °C
実験手順
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.
後処理
- additionAfter the addition
- washThe mixture was washed with water, aqueous 4% sodium bicarbonate, brine
- dry with materialdried over sodium sulphate
- customthe solvent removed under reduced pressure
- customThe residue was purified by column chromatography on silica flash
出典と根拠
- ORDレコード
- ord-f27acf8f24c948bdabc50eece916231a
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07906530B2
関連ノート
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