3,5-Dibromopyridine → 3,5-Dibromopyridine N-oxide
反応式
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Br:8])[CH:7]=1.ClC1C=CC=C(C(OO)=[O:17])C=1>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[N+:4]([O-:17])[CH:5]=[C:6]([Br:8])[CH:7]=1参加物
4
実験手順
3,5-Dibromopyridine 2.37 g is dissolved in methylene chloride 25 ml and thereto is added m-chloroperbenzoic acid 2.96 g at room temperature under stirring. After stirring for 5 hours at room temperature, additional m-chloroperbenzoic acid 246 mg is added thereto and the mixture is stirred. After 15 hours the solvent is removed in vacuo and the residue is purified by silica gel chromatography (solvent; n-hexane:ethyl acetate=1:1) to give 3,5-dibromopyridine N-oxide as colorless crystals, 2.26 g. mp 140-142° C.
後処理
- stirringAfter stirring for 5 hours at room temperature
- stirringthe mixture is stirred
- customAfter 15 hours the solvent is removed in vacuo
- customthe residue is purified by silica gel chromatography (solvent; n-hexane:ethyl acetate=1:1)
出典と根拠
- ORDレコード
- ord-4588c7ebedeb496eb9089a9308afeb58
- 出典データセット
- uspto-grants-2007_09
- 特許番号
- US07273868B2
反応ノート
読み込み中…