Methanol → HCID 178526243、化合物
反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[NH:12]1[C:16]2=[N:17][CH:18]=[CH:19][CH:20]=[C:15]2[CH:14]=[CH:13]1.CO>ClCCl>[NH:12]1[C:16]2=[N+:17]([O-:9])[CH:18]=[CH:19][CH:20]=[C:15]2[CH:14]=[CH:13]1参加物
5
反応条件
- 温度
- 0 °C
実験手順
539.7 g (2.35 mol) of 3-chloroperbenzoic acid are dissolved in 6.11 l of dichloromethane, and water that separates off is removed. The organic phase is dried over sodium sulfate and cooled to 0° C. A solution of 163 g (1.38 mol) of 1H-pyrrolo[2,3-b]pyridine in 1.00 l of dichloromethane is then added, and the temperature is allowed to increase to room temperature. After 2 hours, sufficient methanol to re-dissolve the precipitate formed is added. The mixture is filtered through silica gel (mobile phase: dichloromethane/methanol 95:5) and the product fractions are dried after concentration under high vacuum.
後処理
- customwater that separates off is removed
- dry with materialThe organic phase is dried over sodium sulfate
- temperatureto increase to room temperature
- customformed
- additionis added
- filtrationThe mixture is filtered through silica gel (mobile phase: dichloromethane/methanol 95:5)
- customthe product fractions are dried
- concentrationafter concentration under high vacuum
出典と根拠
- ORDレコード
- ord-9895e424d20e49a3b999223b13d4f924
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737153B2
反応ノート
読み込み中…