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

HRID 69314

반응식

HRID 69314 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-04113bd597ee43be87c8b0ace7ac50f1
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822494B2

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