m-Chloroperbenzoic acid → 2-Chloro-5-methoxy-3-methylpyridine 1-oxide

HRID 69314

反応式

HRID 69314 の反応式
ClC1C=C(C=CC=1)C(OO)=[O:6].[Cl:12][C:13]1[C:18]([CH3:19])=[CH:17][C:16]([O:20][CH3:21])=[CH:15][N:14]=1>ClCCl>[Cl:12][C:13]1[C:18]([CH3:19])=[CH:17][C:16]([O:20][CH3:21])=[CH:15][N+:14]=1[O-:6]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 128520162-Chloro-5-methoxy-3-methylpyridine

生成物 1

HCID 867178152-Chloro-5-methoxy-3-methylpyridine 1-oxide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-Chloroperoxybenzoic acid (70%, 695 mg, 2.82 mmol) was added to a solution of 2-chloro-5-methoxy-3-methylpyridine (370 mg, 2.35 mmol) in dichloromethane (10 mL). After stirring for 18 hours at room temperature, the reaction mixture was concentrated in vacuo and purified via silica gel chromatography (Gradient: 0% to 10% methanol in ethyl acetate) to afford the product as a white solid. Yield: 370 mg, 2.13 mmol, 91%. 1H NMR (400 MHz, CD3OD) δ 8.14 (d, J=2.5 Hz, 1H), 7.23 (d, J=2.3 Hz, 1H), 3.88 (s, 3H), 2.44 (s, 3H).

後処理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. custompurified via silica gel chromatography (Gradient: 0% to 10% methanol in ethyl acetate)

出典と根拠

ORDレコード
ord-04113bd597ee43be87c8b0ace7ac50f1
出典データセット
uspto-grants-2014_09
特許番号
US08822494B2

関連ノート

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