m-Chloroperbenzoic acid → 5-Bromo-2-(2-methyl-2H-tetrazol-5-yl)pyridine 1-oxide

HRID 1782090ノート

反応式

HRID 1782090 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:9]=[N:10][N:11]([CH3:13])[N:12]=2)=[N:6][CH:7]=1.ClC1C=CC=C(C(OO)=[O:22])C=1>ClCCCl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:9]=[N:10][N:11]([CH3:13])[N:12]=2)=[N+:6]([O-:22])[CH:7]=1

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 234386535-Bromo-2-(2-methyl-2H-tetrazol-5-yl)pyridine

生成物 1

HCID 690650085-Bromo-2-(2-methyl-2H-tetrazol-5-yl)pyridine 1-oxide

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
80 °C

実験手順

5-Bromo-2-(2-methyl-2H-tetrazol-5-yl)pyridine (175 mg, 0.73 mM) and 3-chloroperbenzoic acid (wet, 70%: 0.50 g, 2.05 mM) were dissolved in 1,2-dichloroethane (5 ml) and heated at 80° C. for 1.5 hours. The mixture was submitted directly to silica gel chromatography, eluting with 25% acetonitrile in dichloromethane. 5-Bromo-2-(2-methyl-2H-tetrazol-5-yl)pyridine 1-oxide was thus obtained as a white solid (165 mg). This material was homogeneous by tlc analysis and was used in the subsequent step without further characterization or purification.

後処理

  1. washeluting with 25% acetonitrile in dichloromethane

出典と根拠

ORDレコード
ord-1ec23d976acb4f869970ee250c87a048
出典データセット
uspto-grants-2009_03
特許番号
US07498350B2

反応ノート

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