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

HRID 1782090노트

반응식

HRID 1782090 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  1. washeluting with 25% acetonitrile in dichloromethane

출처 및 근거

ORD 기록
ord-1ec23d976acb4f869970ee250c87a048
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07498350B2

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