m-Chloroperbenzoic acid → HCID 178507188、化合物
反応式
C1C=C(Cl)C=C(C(OO)=[O:9])C=1.[Br:12][C:13]1[C:14]([NH2:19])=[N:15][CH:16]=[CH:17][CH:18]=1>CC(C)=O>[NH2:19][C:14]1[C:13]([Br:12])=[CH:18][CH:17]=[CH:16][N+:15]=1[O-:9]参加物
4
反応条件
- 温度
- 23 °C
実験手順
mCPBA (12.0 g, 69.3 mmol) was added portionwise over 5 min to a solution of 3-bromopyridin-2-amine (10 g, 58 mmol) in anhydrous acetone (150 mL) at 0° C. The resulting mixture was warmed to 23° C. and stirred for 1 h, then concentrated. The residue was partitioned between a solution of 5% methanol in chloroform and saturated aqueous sodium hydroxide solution (3×). The combined organic layers were washed with brine, dried over anhydrous sodium sulfate, and concentrated to give the title compound. MS: m/z=189.0 (M+1).
後処理
- concentrationconcentrated
- customThe residue was partitioned between a solution of 5% methanol in chloroform and saturated aqueous sodium hydroxide solution (3×)
- washThe combined organic layers were washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-0af1ba88a13c40cf9271a89f2638e8d5
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09296750B2
反応ノート
読み込み中…