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

HRID 2278818

Reaktionsgleichung

Reaktionsgleichung von HRID 2278818
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]

Komponenten

4

Edukt 2

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

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-a86046c0d8fa4e89a9cf9a4b3d8e5687
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09133190B2

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